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Sample records for preparation phase represents

  1. Preparation of single phase molybdenum boride

    International Nuclear Information System (INIS)

    Camurlu, Hasan Erdem

    2011-01-01

    Highlights: → Formation of Mo and a mixture of molybdenum boride phases take place in preparation of molybdenum borides. → It is intricate to prepare single phase molybdenum borides. → Formation of single phase MoB from MoO 3 + B 2 O 3 + Mg mixtures has not been reported previously. → Single phase MoB was successfully prepared through a combination of mechanochemical synthesis and annealing process. - Abstract: The formation of MoB through volume combustion synthesis (VCS), and through mechanochemical synthesis (MCS) followed by annealing has been investigated. MoO 3 , B 2 O 3 and Mg were used as reactants while MgO and NaCl were introduced as diluents. Products were leached in dilute HCl solution and were subjected to X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM) examinations. Mo was the major phase component in the VCS products under all the experimental conditions. Mo 2 B, MoB, MoB 2 and Mo 2 B 5 were found as minor phases. Products of MCS contained a mixture of Mo 2 B, MoB, MoB 2 and Mo. After annealing the MCS product at 1400 deg. C for 3 h, single phase α-MoB was obtained.

  2. Preparation phase of Mochovce NPP unit 3 and 4 construction completion

    International Nuclear Information System (INIS)

    Cillik, I.; Tvaroska, V.; Liska, P.; Ziman, V.

    2005-01-01

    In this presentation authors deal with preparation phase of Mochovce NPP unit 3 and 4 construction completion. The preparation phase of the Mochovce unit 3 and 4 construction completion gives following main outputs: (a) Detail Safety Concept gives definitive complex safety and technical improvement of MO34, more precise analysis of the total cost of construction completion, a list of potential suppliers and construction completion time schedule; (b) Appendices of Basic Design Documentation and Preliminary SAR serves as basic documentation for UJD SR decision making according to Law No. 541 for start of Realization Phase; (c) The Preparation Phase represents effective tool for start of MO34 construction completion Realization Phase.

  3. Condensed phase preparation of 2,3-pentanedione

    Science.gov (United States)

    Miller, D.J.; Perry, S.M.; Fanson, P.T.; Jackson, J.E.

    1998-11-03

    A condensed phase process for the preparation of purified 2,3-pentanedione from lactic acid and an alkali metal lactate is described. The process uses elevated temperatures between about 200 to 360 C for heating a reaction mixture of lactic acid and an alkali metal lactate to produce the 2,3-pentanedione in a reaction vessel. The 2,3-pentanedione produced is vaporized from the reaction vessel and condensed with water. 5 figs.

  4. Sampling device for withdrawing a representative sample from single and multi-phase flows

    Science.gov (United States)

    Apley, Walter J.; Cliff, William C.; Creer, James M.

    1984-01-01

    A fluid stream sampling device has been developed for the purpose of obtaining a representative sample from a single or multi-phase fluid flow. This objective is carried out by means of a probe which may be inserted into the fluid stream. Individual samples are withdrawn from the fluid flow by sampling ports with particular spacings, and the sampling parts are coupled to various analytical systems for characterization of the physical, thermal, and chemical properties of the fluid flow as a whole and also individually.

  5. Nonequilibrium phase formation in oxides prepared at low temperature: Fergusonite-related phases

    International Nuclear Information System (INIS)

    Mather, S.A.; Davies, P.K.

    1995-01-01

    Sol-gel methods have been developed to prepare YNbO 4 , YTaO 4 , and other rare-earth niobates and tantalates with fergusonite-related crystal structures. At low temperatures, all of the fergusonites, with the exception of SmTaO 4 , crystallize in a metastable tetragonal (T') structure similar to that of tetragonal zirconia. Although all of the equilibrium forms of these oxides adopt a crystal structure containing an ordered distribution of the trivalent and pentavalent cations, a random cation distribution is obtained in the metastable T' phase. Metastable phase formation is often ascribed solely to kinetically limited topotactic crystallization. However, the changes in the grain size and unit-cell volumes that accompany the metastable-to-equilibrium fergusonite conversions imply that other physical phenomena induced by small-particle synthesis, namely the Gibbs-Thompson pressure effect and the increased contribution of surface energy, cannot be ignored

  6. CARDfile data base representativeness, Phase 1 : general characteristics including populations, vehicles, roads, and fatal accidents

    Science.gov (United States)

    1988-08-01

    This report details the results of an analysis performed to evaluate the : representativeness of the Crash Avoidance Research accident data base : (CARDfile). The accident records for 1983 and 1984 from six states (Indiana, : Maryland, Michigan, Penn...

  7. CARDfile Data Base Representatives - Phase I: General Characteristics including Populations, Vehicles, Roads, and Fatal Accidents

    Science.gov (United States)

    1985-12-01

    This report details the results of an analysis performed to evaluate the representativeness of the Crash Avoidance Research accident data base (CARDfile). The accident records for 1983 and 1984 from six states (Indiana, Maryland, Michigan, Pennsylvan...

  8. The Cell Cycle: An Activity Using Paper Plates to Represent Time Spent in Phases of the Cell Cycle

    Science.gov (United States)

    Scherer, Yvette D.

    2014-01-01

    In this activity, students are given the opportunity to combine skills in math and geometry for a biology lesson in the cell cycle. Students utilize the data they collect and analyze from an online onion-root-tip activity to create a paper-plate time clock representing a 24-hour cell cycle. By dividing the paper plate into appropriate phases of…

  9. The majority of patients with metastatic melanoma are not represented in pivotal phase III immunotherapy trials

    DEFF Research Database (Denmark)

    Donia, Marco; Kimper-Karl, Marie Louise; Høyer, Katrine Lundby

    2017-01-01

    BACKGROUND: Recent randomised phase III trials have led to the approval of several immune checkpoint inhibitors for unresectable or metastatic melanoma (MM). These trials all employed strict patient selection criteria, and it is currently unknown how large proportion of 'real-world' patients diag...... a huge knowledge gap regarding the usefulness of new immunotherapies in the 'real-world' patient population, and urge additional testing of known regimens in selected poor prognosis cohorts.......BACKGROUND: Recent randomised phase III trials have led to the approval of several immune checkpoint inhibitors for unresectable or metastatic melanoma (MM). These trials all employed strict patient selection criteria, and it is currently unknown how large proportion of 'real-world' patients...... in 2014, were included in the analysis. Seven pre-defined eligibility criteria, all used to select patients for enrolment in five recent randomised phase III immunotherapy trials, were analysed. RESULTS: Fifty-five percent of the total population with MM did not meet one or more eligibility criteria ('not...

  10. A Local Condensation Analysis Representing Two-phase Annular Flow in Condenser/radiator Capillary Tubes

    Science.gov (United States)

    Karimi, Amir

    1991-01-01

    NASA's effort for the thermal environmental control of the Space Station Freedom is directed towards the design, analysis, and development of an Active Thermal Control System (ATCS). A two phase, flow through condenser/radiator concept was baselined, as a part of the ATCS, for the radiation of space station thermal load into space. The proposed condenser rejects heat through direct condensation of ATCS working fluid (ammonia) in the small diameter radiator tubes. Analysis of the condensation process and design of condenser tubes are based on the available two phase flow models for the prediction of flow regimes, heat transfer, and pressure drops. The prediction formulas use the existing empirical relationships of friction factor at gas-liquid interface. An attempt is made to study the stability of interfacial waves in two phase annular flow. The formulation is presented of a stability problem in cylindrical coordinates. The contribution of fluid viscosity, surface tension, and transverse radius of curvature to the interfacial surface is included. A solution is obtained for Kelvin-Helmholtz instability problem which can be used to determine the critical and most dangerous wavelengths for interfacial waves.

  11. Phase transitions in PZT ceramics prepared by different techniques

    Czech Academy of Sciences Publication Activity Database

    Deineka, Alexander; Suchaneck, G.; Jastrabík, Lubomír; Gerlach, G.

    2002-01-01

    Roč. 41, 11B (2002), s. 6966-6968 ISSN 0021-4922 R&D Projects: GA MŠk LN00A015 Institutional research plan: CEZ:AV0Z1010914 Keywords : PZT * phase transitions * band gap * ferroelectrics Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.280, year: 2002

  12. Preparation and sintering of Zr(C,N,O) phases

    International Nuclear Information System (INIS)

    Tamborenea, S.; Mazzoni, A.D.; Aglietti, E.F.

    2003-01-01

    The Zr(C,O,N) compounds form a great mono-phase zone belonging to the pseudoternary ZrO-ZrN-ZrC system.Theses phases have cubic crystalline structure with a o parameter depending on the C, O 2 and N 2 content.These phases have many potential applications in the manufacture of ceramic pieces utilizable as electronic conductors.The Zr (C,O,N) phases can be obtained from ZrO 2 by carbonitriding reactions: that is carbothermal reduction and simultaneous nitriding.In this work a series of experiences of carbonitriding of zirconia under different conditions (temperatures between 1400 and 1600degC, times of 120 min, carbon content between 20 and 40%) in order to obtain suitable powders to be sintered.The XRD analysis shows the Zr(C,O,N) as the main products and β -ZrON as the only secondary product in proportions depending on the obtaining conditions.The variables employed were the C content and the reaction temperature.The Zr(C,O,N) content varies between 40 and 90% and tends to increase with the temperature and the carbon content whereas the β -ZrON phase varies between the 40 and 10 % decreasing its proportion with temperature and the carbon content.The oxidation resistance of these phases was studied by DTA-TG tests in air.Results show complete oxidation reaction at ∼500degC in air.The sintering of these materials was made on disks obtained by pressing of powders of Zr(C,N,O) contents higher than 90%.Sintering was performed in nitrogen atmosphere and temperatures between 1450 and 1620degC.Disks were characterized by pycnometry and Hg volumeter.The densities obtained were between 5 and 6,6g/cm 3 with a tendency to increase with the Zr(C,N,O) phase content, the temperature and the sintering time.Sintered disks were characterized by dilatometry in N 2

  13. Preparation and Characterization of Membranes Formed by Nonsolvent Induced Phase Separation: A Review

    KAUST Repository

    Guillen, Gregory R.; Pan, Yinjin; Li, Minghua; Hoek, Eric M. V.

    2011-01-01

    . The body of knowledge has grown exponentially in the past fifty years, which suggests the need for a critical review of the literature. Here we present a review of nonsolvent induced phase separation membrane preparation and characterization for many

  14. Investigation of representing hysteresis in macroscopic models of two-phase flow in porous media using intermediate scale experimental data

    Science.gov (United States)

    Cihan, Abdullah; Birkholzer, Jens; Trevisan, Luca; Gonzalez-Nicolas, Ana; Illangasekare, Tissa

    2017-01-01

    Incorporating hysteresis into models is important to accurately capture the two phase flow behavior when porous media systems undergo cycles of drainage and imbibition such as in the cases of injection and post-injection redistribution of CO2 during geological CO2 storage (GCS). In the traditional model of two-phase flow, existing constitutive models that parameterize the hysteresis associated with these processes are generally based on the empirical relationships. This manuscript presents development and testing of mathematical hysteretic capillary pressure—saturation—relative permeability models with the objective of more accurately representing the redistribution of the fluids after injection. The constitutive models are developed by relating macroscopic variables to basic physics of two-phase capillary displacements at pore-scale and void space distribution properties. The modeling approach with the developed constitutive models with and without hysteresis as input is tested against some intermediate-scale flow cell experiments to test the ability of the models to represent movement and capillary trapping of immiscible fluids under macroscopically homogeneous and heterogeneous conditions. The hysteretic two-phase flow model predicted the overall plume migration and distribution during and post injection reasonably well and represented the postinjection behavior of the plume more accurately than the nonhysteretic models. Based on the results in this study, neglecting hysteresis in the constitutive models of the traditional two-phase flow theory can seriously overpredict or underpredict the injected fluid distribution during post-injection under both homogeneous and heterogeneous conditions, depending on the selected value of the residual saturation in the nonhysteretic models.

  15. Preparation and characterization of a novel polymeric based solid-solid phase change heat storage material

    International Nuclear Information System (INIS)

    Xi Peng; Gu Xiaohua; Cheng Bowen; Wang Yufei

    2009-01-01

    Here we reported a two-step procedure for preparing a novel polymeric based solid-solid phase change heat storage material. Firstly, a copolymer monomer containing a polyethylene glycol monomethyl ether (MPEG) phase change unit and a vinyl unit was synthesized via the modification of hydrogen group of MPEG. Secondly, by copolymerization of the copolymer monomer and phenyl ethylene, a novel polymeric based solid-solid phase change heat storage material was prepared. The composition, structure and properties of the novel polymeric based solid-solid phase change material were characterized by IR, 1 H NMR, DSC, WAXD, and POM, respectively. The results show that the novel polymeric based solid-solid phase change material possesses of excellent crystal properties and high phase change enthalpy.

  16. Use of solid-phase salt catalysts in furfural preparation

    Energy Technology Data Exchange (ETDEWEB)

    Morozov, E.F.; Shkut, V.M.; Kebich, M.S.; Kuznetsova, T.A.

    1981-01-01

    The manufacture of furfural (I) from tanning waste, birch sawdust, or corncobs at 220-230 degrees in the presence of 2.0-3.0% double superphosphate, ammophos, (NH/sub 4/)/sub 2/SO/sub 4/, NH/sub 4/NO/sub 3/, or NH/sub 4/Cl was evaluated. Most of I is formed within 40 minutes in the presence of NH4NO3 or NH4Cl, and within 55 minutes in the presence of double superphosphate. The highest yield of I was obtained in the presence of NH4NO3 and/or NH4Cl. The solid-phase catalyst caused a little degradation of lignocellulose.

  17. HiLumi prepares its construction phase with industry

    CERN Multimedia

    Agnes Szeberenyi

    2015-01-01

    The High-Luminosity LHC project is now seeking industrial suppliers and collaborations to start the construction phase and make the high-luminosity upgrade happen. The “HiLumi LHC goes to Industry” event held on 26 June aimed to foster R&D collaborations and knowledge exchange between CERN and small and medium-sized enterprises (SMEs) - the perfect opportunity for them to match their capacity with the requirements of HiLumi.   Isabel Bejar-Alonso (High-Luminosity LHC Technical Coordinator) addresses the participants of the “HiLumi LHC goes to Industry” event held at IdeaSquare on 26 June. To reach the 14 TeV and 3000 fb-1 goal of the High-Luminosity LHC, more than 1.2 km of the current LHC machine will need to be replaced with high-technology components that require cutting-edge technologies. HiLumi experts have already identified more than 65 technology areas and even more challenging components that need to be manufactured, assembled and tested bef...

  18. Robust Multiscale Modelling Of Two-Phase Steels On Heterogeneous Hardware Infrastructures By Using Statistically Similar Representative Volume Element

    Directory of Open Access Journals (Sweden)

    Rauch Ł.

    2015-09-01

    Full Text Available The coupled finite element multiscale simulations (FE2 require costly numerical procedures in both macro and micro scales. Attempts to improve numerical efficiency are focused mainly on two areas of development, i.e. parallelization/distribution of numerical procedures and simplification of virtual material representation. One of the representatives of both mentioned areas is the idea of Statistically Similar Representative Volume Element (SSRVE. It aims at the reduction of the number of finite elements in micro scale as well as at parallelization of the calculations in micro scale which can be performed without barriers. The simplification of computational domain is realized by transformation of sophisticated images of material microstructure into artificially created simple objects being characterized by similar features as their original equivalents. In existing solutions for two-phase steels SSRVE is created on the basis of the analysis of shape coefficients of hard phase in real microstructure and searching for a representative simple structure with similar shape coefficients. Optimization techniques were used to solve this task. In the present paper local strains and stresses are added to the cost function in optimization. Various forms of the objective function composed of different elements were investigated and used in the optimization procedure for the creation of the final SSRVE. The results are compared as far as the efficiency of the procedure and uniqueness of the solution are considered. The best objective function composed of shape coefficients, as well as of strains and stresses, was proposed. Examples of SSRVEs determined for the investigated two-phase steel using that objective function are demonstrated in the paper. Each step of SSRVE creation is investigated from computational efficiency point of view. The proposition of implementation of the whole computational procedure on modern High Performance Computing (HPC

  19. Preparation and characterization of sepiolite-based phase change material nanocomposites for thermal energy storage

    International Nuclear Information System (INIS)

    Konuklu, Yeliz; Ersoy, Orkun

    2016-01-01

    Highlights: • Sepiolite-based phase change material nanocomposites were prepared. • An easy direct impregnation process was used. • This paper is one of the first study about sepiolite-based phase change material nanocomposites. • Influence of PCM type on thermal properties of nanocomposites was reported. - Abstract: This paper is one of the first study about the preparation and characterization of sepiolite-based phase change material nanocomposites for thermal energy storage applications. Sepiolite is an important natural fibrous raw material. Nanoscale fibrous tubular structure of sepiolite becomes important in nanocomposite preparation. In this study, sepiolite/paraffin and sepiolite/decanoic acid nanocomposites were manufactured by the direct impregnation method. By the preparation of nanocomposites, PCM move in tubular channels of sepiolite, phase changing occurs in these tubes and surface area increases like as in microencapsulation. The structure and properties of nanocomposites PCMs (CPCM) have been characterized via scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), and Fourier transform infrared spectroscopy (FTIR). The SEM results prove the successful preparation of phase change material/sepiolite nanocomposites and point out that the fibers of sepiolite is modified with phase change materials in the nanocomposite. The phase change enthalpies of melting and freezing were about 62.08 J/g and −62.05 J/g for sepiolite/paraffin nanocomposites and 35.69 J/g and −34.55 J/g for sepiolite/decanoic acid nanocomposites, respectively. The results show that PCM/sepiolite nanocomposites were prepared successfully and their properties are very suitable for thermal energy storage applications.

  20. Jules Horowitz Reactor: Organisation for the Preparation of the Commissioning Phase and Normal Operation

    Energy Technology Data Exchange (ETDEWEB)

    Estrade, J.; Fabre, J. L.; Marcille, O. [French Alternative Energies end Atomic Energy Commission, Provence (France)

    2013-07-01

    The Jules Horowitz Reactor (JHR) is a new modern Material Testing Reactor (MTR) currently under construction at CEA Cadarache research centre in the south of France. It will be a major research facility in support to the development and the qualification of materials and fuels under irradiation with sizes and environment conditions relevant for nuclear power plants in order to optimise and demonstrate safe operations of existing power reactors as well as to support future reactors design. It will represent also an important research infrastructure for scientific studies dealing with material and fuel behaviour under irradiation. The JHR will contribute also to secure the production of radioisotope for medical application. This is a key public health stake. The construction of JHR which started in 2007 is going-on with target of commissioning by the end of 2017. The design of the reactor provides modern experimental capacity in support to R and D programs for the nuclear energy for the next 60 years. In parallel to the facility construction, the preparation of the future staff and of the organisation to operate the reactor safely, reliably and efficiently is an important issue. In this framework, many actions are in progress to elaborate: Ο the staffing and the organisational structure for the commissioning test phases and also for normal operation, Ο the documentation in support to the reactor operation (safety analysis report, general operating rules, procedures, instructions, ···), Ο the maintenance, in service and periodic test programs, Ο staff training programs by using dedicated facilities (simulator, ···) Ο commissioning test programs for ensuring that the layout of systems and subcomponents is completed in accordance with the design requirements, the specification performances and the safety criteria. These commissioning tests will also be helpful for transferring the knowledge on the installed systems to the operating group. This paper gives the

  1. Domestic Consequences of United States Population Change. Report Prepared by the Select Committee on Population, U.S. House of Representatives, Ninety-Fifth Congress, Second Session.

    Science.gov (United States)

    Congress of the U.S., Washington, DC. House Select Committee on Population.

    The report, prepared by the Select Committee on Population of the United States House of Representatives, discusses the consequences of the changing age composition and geographical distribution of the population. The committee recommends that the government needs to anticipate these changes in order to develop a policy in response to the problems…

  2. Local preparation and evaluation of liquid phase radioimmunoassay for determination of human serum cortisol

    International Nuclear Information System (INIS)

    Sallam, Kh.M.; El-Bayoumy, A.S.A.; Ebeid, N.H.; Michael, E.; Zein, N.; Elfarargy, Ah.F.

    2017-01-01

    The main objective of the present study was the preparation of the primary reagents of cortisol radioimmunoassay (RIA) using liquid phase double antibody technique. Three basic components were prepared and characterized to obtain valid and accurate system. These components were polyclonal anti-cortisol antibody, "1"2"5I-cortisol RIA tracer and cortisol standards. Cortisol requires conjugation step to be real antigen. Therefore, in this study this mandatory conjugation step was performed & characterized. Then formulation, optimization and validation of this liquid phase RIA technique were carried out. This assay is precise, specific and sensitive enough for using as a diagnostic tool for the adrenal cortex status. (author)

  3. Facile preparation of an alternating copolymer-based high molecular shape-selective organic phase for reversed-phase liquid chromatography.

    Science.gov (United States)

    Mallik, Abul K; Noguchi, Hiroki; Rahman, Mohammed Mizanur; Takafuji, Makoto; Ihara, Hirotaka

    2018-06-22

    The synthesis of a new alternating copolymer-grafted silica phase is described for the separation of shape-constrained isomers of polycyclic aromatic hydrocarbons (PAHs) and tocopherols in reversed-phase high-performance liquid chromatography (RP-HPLC). Telomerization of the monomers (octadecyl acrylate and N-methylmaleimide) was carried out with a silane coupling agent; 3-mercaptopropyltrimethoxysilane (MPS), and the telomer (T) was grafted onto porous silica surface to prepare the alternating copolymer-grafted silica phase (Sil-alt-T). The new hybrid material was characterized by elemental analyses, diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy, and solid-state 13 C and 29 Si cross-polarization magic-angle spinning (CP/MAS) NMR spectroscopy. The results of 13 C CP/MAS NMR demonstrated that the alkyl chains of the grafted polymers in Sil-alt-T remained disordered, amorphous, and mobile represented by gauche conformational form. Separation abilities and molecular-shape selectivities of the prepared organic phase were evaluated by the separation of PAHs isomers and Standard Reference Material 869b, Column Selectivity Test Mixture for Liquid Chromatography, respectively and compared with commercially available octadecylsilylated silica (ODS) and C 30 columns as well as previously reported alternating copolymer-based column. The effectiveness of this phase is also demonstrated by the separation of tocopherol isomers. Oriented functional groups along the polymer main chains and cavity formations are investigated to be the driving force for better separation with multiple-interactions with the solutes. One of the advantages of the Sil-alt-T phase to that of the previously reported phase is the synthesis of the telomer first and then immobilized onto silica surface. In this case, the telomer was characterized easily with simple spectroscopic techniques and the molecular mass and polydispersity index of the telomer were determined by size exclusion

  4. Aqueous preparation of polyethylene glycol/sulfonated graphene phase change composite with enhanced thermal performance

    International Nuclear Information System (INIS)

    Li, Hairong; Jiang, Ming; Li, Qi; Li, Denian; Chen, Zongyi; Hu, Waping; Huang, Jing; Xu, Xizhe; Dong, Lijie; Xie, Haian; Xiong, Chuanxi

    2013-01-01

    Highlights: • We report an aqueous preparation technique of PEG/graphene phase change composite. • Hydrophilic sulfonated graphene (SG) nanosheets were synthesized. • Large increase in thermal conductivity is attained at low SG loading. • High latent heat is retained due to the low filler loading. • Affinity between SG and PEG contributes to the enhanced thermal performance. - Abstract: A polyethylene glycol (PEG)/sulfonated graphene (SG) phase change composite with enhanced thermal performance was prepared by solution processing in aqueous medium. It is remarkable that the addition of only 4 wt.% of SG to PEG could lead to a four times higher increase in thermal conductivity and a slight decrease in the phase change enthalpy, which is attributed to the formation of efficient thermal conductive network within the PEG matrix relevant to the excellent thermal property and unique 2-dimensional morphology of graphene as well as strong interface affinity between PEG matrix and SG nanosheets. The aqueous preparation technique is expected to pioneer a new way to prepare environment friendly organic phase change materials, and the production of PEG/SG composites is potentially scalable due to the facile fabricating process

  5. Preparing poly (caprolactone) micro-particles through solvent-induced phase separation

    DEFF Research Database (Denmark)

    Li, Xiaoqiang; Kanjwal, Muzafar Ahmed; Stephansen, Karen

    2012-01-01

    Poly (caprolactone) (PCL) particles with the size distribution from 1 to 100 μm were prepared through solvent-induced phase separation, in which polyvinyl-alcohol (PVA) was used as the matrix-forming polymer to stabilize PCL particles. The cloud point data of PCL-acetone-water was determined...

  6. Membranes Prepared by Self-assembly and Chelation Assisted Phase Inversion

    KAUST Repository

    Xie, Yihui

    2017-05-19

    We combine self-assembly in solution, complexation with metallic salts and phase separation induced by solvent-non-solvent exchange to prepare nanostructured membranes for separation in the nanofiltration range. The method was applied to synthesized poly(acrylic acid)-b-polysulfone-b-poly(acrylic acid) copolymers dissolved in a selective solvent mixture and immersed in aqueous Cu2+ or Ag+ solutions.

  7. Membranes Prepared by Self-assembly and Chelation Assisted Phase Inversion

    KAUST Repository

    Xie, Yihui; Sutisna, Burhannudin; Nunes, Suzana Pereira

    2017-01-01

    We combine self-assembly in solution, complexation with metallic salts and phase separation induced by solvent-non-solvent exchange to prepare nanostructured membranes for separation in the nanofiltration range. The method was applied to synthesized poly(acrylic acid)-b-polysulfone-b-poly(acrylic acid) copolymers dissolved in a selective solvent mixture and immersed in aqueous Cu2+ or Ag+ solutions.

  8. Microstructure Optimization of Dual-Phase Steels Using a Representative Volume Element and a Response Surface Method: Parametric Study

    Science.gov (United States)

    Belgasam, Tarek M.; Zbib, Hussein M.

    2017-12-01

    Dual-phase (DP) steels have received widespread attention for their low density and high strength. This low density is of value to the automotive industry for the weight reduction it offers and the attendant fuel savings and emission reductions. Recent studies on developing DP steels showed that the combination of strength/ductility could be significantly improved when changing the volume fraction and grain size of phases in the microstructure depending on microstructure properties. Consequently, DP steel manufacturers are interested in predicting microstructure properties and in optimizing microstructure design. In this work, a microstructure-based approach using representative volume elements (RVEs) was developed. The approach examined the flow behavior of DP steels using virtual tension tests with an RVE to identify specific mechanical properties. Microstructures with varied martensite and ferrite grain sizes, martensite volume fractions, carbon content, and morphologies were studied in 3D RVE approaches. The effect of these microstructure parameters on a combination of strength/ductility of DP steels was examined numerically using the finite element method by implementing a dislocation density-based elastic-plastic constitutive model, and a Response surface methodology to determine the optimum conditions for a required combination of strength/ductility. The results from the numerical simulations are compared with experimental results found in the literature. The developed methodology proves to be a powerful tool for studying the effect and interaction of key microstructural parameters on strength and ductility and thus can be used to identify optimum microstructural conditions.

  9. Nanocasting of Periodic Mesoporous Materials as an Effective Strategy to Prepare Mixed Phases of Titania

    Directory of Open Access Journals (Sweden)

    Luther Mahoney

    2015-12-01

    Full Text Available Mesoporous titanium dioxide materials were prepared using a nanocasting technique involving silica SBA-15 as the hard-template. At an optimal loading of titanium precursor, the hexagonal periodic array of pores in SBA-15 was retained. The phases of titanium dioxide could be easily varied by the number of impregnation cycles and the nature of titanium alkoxide employed. Low number of impregnation cycles produced mixed phases of anatase and TiO2(B. The mesoporous TiO2 materials were tested for solar hydrogen production, and the material consisting of 98% anatase and 2% TiO2(B exhibited the highest yield of hydrogen from the photocatalytic splitting of water. The periodicity of the pores was an important factor that influenced the photocatalytic activity. This study indicates that mixed phases of titania containing ordered array of pores can be prepared by using the nanocasting strategy.

  10. Preparation and characterization of novel anion phase change heat storage materials.

    Science.gov (United States)

    Hong, Wei; Lil, Qingshan; Sun, Jing; Di, Youbo; Zhao, Zhou; Yu, Wei'an; Qu, Yuan; Jiao, TiFeng; Wang, Guowei; Xing, Guangzhong

    2013-10-01

    In this paper, polyurethane phase change material was successfully prepared with TDI with BDO for hard segments and PEG for soft segments. Moreover, based on this the solid-solid phase change material, A-PCM1030 which can release anions was prepared with the successful addition of anion additives A1030 for the first time. Then the test of the above material was conducted utilizing FT-IR, DSC, TEM, WAXD and Air Ion Detector. The Results indicated that the polyurethane phase change material possesses excellent thermal stability since there was no appearance of liquid leakage and phase separation after 50 times warming-cooling thermal cycles. It also presented reversibility on absorbing and releasing heat. In addition, adding a little A1030 can increase the thermal stability and reduce phase transition temperatures, as well as reduce the undercooling of the polyurethane phase change material. In addition, the anion test results suggested that the supreme amount of anion released by A-PCM1030 could reach 2510 anions/cm3 under dynamic conditions, which is beneficial for human health.

  11. Sample preparation with solid phase microextraction and exhaustive extraction approaches: Comparison for challenging cases.

    Science.gov (United States)

    Boyacı, Ezel; Rodríguez-Lafuente, Ángel; Gorynski, Krzysztof; Mirnaghi, Fatemeh; Souza-Silva, Érica A; Hein, Dietmar; Pawliszyn, Janusz

    2015-05-11

    In chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample. Various sample preparation strategies have been developed based on exhaustive or non-exhaustive extraction of analytes from matrices. Undoubtedly, amongst all sample preparation approaches, liquid extraction, including liquid-liquid (LLE) and solid phase extraction (SPE), are the most well-known, widely used, and commonly accepted methods by many international organizations and accredited laboratories. Both methods are well documented and there are many well defined procedures, which make them, at first sight, the methods of choice. However, many challenging tasks, such as complex matrix applications, on-site and in vivo applications, and determination of matrix-bound and free concentrations of analytes, are not easily attainable with these classical approaches for sample preparation. In the last two decades, the introduction of solid phase microextraction (SPME) has brought significant progress in the sample preparation area by facilitating on-site and in vivo applications, time weighted average (TWA) and instantaneous concentration determinations. Recently introduced matrix compatible coatings for SPME facilitate direct extraction from complex matrices and fill the gap in direct sampling from challenging matrices. Following introduction of SPME, numerous other microextraction approaches evolved to address limitations of the above mentioned techniques. There is not a single method that can be considered as a universal solution for sample preparation. This review aims to show the main advantages and limitations of the above mentioned sample

  12. Preparation and Characterization of Membranes Formed by Nonsolvent Induced Phase Separation: A Review

    KAUST Repository

    Guillen, Gregory R.

    2011-04-06

    The methods and mechanisms of nonsolvent induced phase separation have been studied for more than fifty years. Today, phase inversion membranes are widely used in numerous chemical industries, biotechnology, and environmental separation processes. The body of knowledge has grown exponentially in the past fifty years, which suggests the need for a critical review of the literature. Here we present a review of nonsolvent induced phase separation membrane preparation and characterization for many commonly used membrane polymers. The key factors in membrane preparation discussed include the solvent type, polymer type and concentration, nonsolvent system type and composition, additives to the polymer solution, and film casting conditions. A brief introduction to membrane characterization is also given, which includes membrane porosity and pore size distribution characterization, membrane physical and chemical properties characterization, and thermodynamic and kinetic evaluation of the phase inversion process. One aim of this review is to lay out the basics for selecting polymer solvent nonsolvent systems with appropriate film casting conditions to produce membranes with the desired performance, morphology, and stability, and to choose the proper way to characterize these properties of nonsolvent induced phase inversion membranes. © 2011 American Chemical Society.

  13. Preparation and Characterization of Modified Montmorillonite/Paraffin Phase Change Microcapsules for Energy Storage

    Directory of Open Access Journals (Sweden)

    LIN Sen

    2017-03-01

    Full Text Available The phase change microcapsules of modified montmorillonite/paraffin were prepared by Pickering emulsion method. Analytic techniques of optical microscopy, scanning electron microscopy(SEM, infrared spectroscopy(FTIR, differential scanning calorimetry(DSC and thermogravimetry(TG were utilized for characterizing chemical structure, morphology and thermal properties. Results show that modified montmorillonite as a new type wall material has excellent performance for protecting core material of paraffin. FTIR spectra of phase change of modified montmorillonite/paraffin microcapsules shows that their characteristic peaks match with corresponding peaks of pure paraffin and modified montmorillonite. DSC results indicate that modified montmorillonite/paraffin microcapsules have similar solid-liquid phase change temperature with pure paraffin. The phase transition enthalpy values of microcapsules with paraffin contents varying from 55% to 80% are 110.5-147.2J/g, indicating that microcapsules have excellent thermal storage performance and the phase change properties can be adjusted by changing contents of paraffin. TG results confirm that modified montmorillonite/paraffin microcapsules have outstanding thermal stability. The presented study indicates that modified montmorillonite is a suitable wall material for preparing paraffin microcapsule. Modified montmorillonite/paraffin microcapsules have advantages of low cost and high performance with a great application potential in the field of thermal storage.

  14. Preparation of 147Pm metal and the determination of the melting point and phase transformation temperatures

    International Nuclear Information System (INIS)

    Angelini, P.; Adair, H.L.

    1976-07-01

    The promethium metal used in the determination of the melting point and phase transformation temperatures was prepared by reduction of promethium oxide with thorium metal at 1600 0 C and distilling the promethium metal into a quartz dome. The melting point and phase transformation temperatures of promethium metal were found to be 1042 +- 5 0 C and 890 +- 5 0 C, respectively. The ratio for the heat of the high-temperature transformation to the heat of fusion was determined to be 0.415

  15. Phase study of titanium dioxide nanoparticle prepared via sol-gel process

    Science.gov (United States)

    Oladeji Araoyinbo, Alaba; Bakri Abdullah, Mohd Mustafa Al; Salleh, Mohd Arif Anuar Mohd; Aziz, Nurul Nadia Abdul; Iskandar Azmi, Azwan

    2018-03-01

    In this study, titanium dioxide nanoparticles have been prepared via sol-gel process using titanium tetraisopropoxide as a precursor with hydrochloric acid as a catalyst, and ethanol with deionized water as solvents. The value of pH used is set to 3, 7 and 8. The sols obtained were dried at 100 °C for 1 hr and calcined at 350, 550, and 750 °C for 3 hrs to observe the phase transformation of titanium dioxide nanoparticle. The samples were characterized by x-ray diffraction and field emission scanning electron microscope. The morphology analysis is obtained from field emission scanning electron microscope. The phase transformation was investigated by x-ray diffraction. It was found that the pH of the solution affect the agglomeration of titanium dioxide particle. The x-ray diffraction pattern of titanium dioxide shows the anatase phase most abundant at temperature of 350 °C. At temperature of 550 °C the anatase and rutile phase were present. At temperature of 750 °C the rutile phase was the most abundant for pH 3, 7 and 8. It was confirmed that at higher temperature the rutile phase which is the stable phase are mostly present.

  16. Structural and morphological characterization of fullerite crystals prepared from the vapor phase

    International Nuclear Information System (INIS)

    Haluska, M.; Fejdi, P.; Vybornov, M.; Kuzmany, H.

    1993-01-01

    Crystal structure, habits and surface structures of fullerite crystals prepared from vapor phase were characterized by X-ray analysis, interfacial angle measurements and optical and scanning electron microscopy (SEM). The study of selected C 60 crystals confirmed the fcc structure at room temperature. The crystal habit is determined by two types of morphological faces, namely {100} and {111}. SEM was used for the observation of thermal etched surfaces. (orig.)

  17. Procedure for the preparation of catalysts for application in catalytic gas phase reactions

    International Nuclear Information System (INIS)

    1976-01-01

    The invention describes the preparation of catalysts to be used in catalytic reactions in the gaseous phase. The catalytic material is disposed at the surface of a ceramic or carbon substrate (av. particle size 0.1 μ - 0.5 cm, surface area smaller than 20 m 2 /g) by bombardment of the catalytic material (Pt, Rh, Pd, Ru, Os, Ir) with energetic ions (Ne, Ar, Kr, Xe) in the vicinity of the substrate in medium vacuum

  18. Improved Procedure for Preparation of Covalently Bonded Cellulose Tris-phenylcarbamate Chiral Stationary Phases

    Institute of Scientific and Technical Information of China (English)

    秦峰; 陈小明; 刘月启; 邹汉法; 王俊德

    2005-01-01

    The classical method for preparation of covalently boned cellulose derivative chiral stationary phases (CSP) with diisocyanate as spacer was improved. Diisocyanate was firstly allowed to react with 3-aminopropyltriethoxysilane, and the resulting product was then applied as the spacer reagent to immobilize cellulose derivatives onto silica gel. Influences of the amount and the length of the spacer on the optical resolution ability of the CSP were investigated. Comparing improved procedure to classical diisocyanate method, the cross-linking between the glucose units of the cellulose derivatives was avoided to the most extent. With the improved procedure, regio-nonselective ways could be adooted to prepare covalently bonded CSP, which showed an advantage for the rapid preparation.

  19. Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

    Science.gov (United States)

    Prosen, Helena

    2014-05-23

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  20. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  1. Local Preparation and Evaluation of Double - antibody Liquid Phase Radioimmunoassay System for Detection of Human Testosterone

    International Nuclear Information System (INIS)

    Shafik, H.M.; Sallam, Kh.M.; Ebeid, N.H.; Elshaer, M.R.; Elshae, M.R.

    2016-01-01

    Preparation, evaluation and optimization of testosterone radioimmunoassay (RIA) system using liquid phase double antibody is considered to be the main objective. Three primary components were prepared and characterized to obtain valid and accurate system. These components were polyclonal testosterone antibody, the "1"2"5I-testosterone tracer and set of testosterone standards. The production of polyclonal testosterone antibody was undertaken by immunizing two groups of females white New-Zealand rabbits with testosterone-3-(O-carboxy methyloxime): BSA as immunogen through primary immunization and five boosters. Both R 1 and R 4 gave anti-serum has a high immuno reactivity. The preparation of "1"2"5I-testosterone tracer was carried out using three different conjugates (testosterone-3-TME, testosterone-3-histamine and testosterone-3-BSA) by electrophilic substitution mechanism using chloramine-T as oxidizing agent. Tracers were characterized in terms of radiochemical yield %, radiochemical purity %, specific activity and immuno reactivity. A set of testosterone standards were prepared using highly purified testosterone antigen. Optimization and validation tests of the local liquid phase RIA system were carried out. In conclusion, the results showed that, the local testosterone RIA system is sensitive, specific and accurate with significant cost reduction in comparison with commertial kit and extended use of the method for routine investigation of variety of diseases especially hypogonadism and associated male infertility

  2. Preparation and thermal conductivity enhancement of composite phase change materials for electronic thermal management

    International Nuclear Information System (INIS)

    Wu, Weixiong; Zhang, Guoqing; Ke, Xiufang; Yang, Xiaoqing; Wang, Ziyuan; Liu, Chenzhen

    2015-01-01

    Highlights: • A kind of composite phase change material board (PCMB) is prepared and tested. • PCMB presents a large thermal storage capacity and enhanced thermal conductivity. • PCMB displays much better cooling effect in comparison to natural air cooling. • PCMB presents different cooling characteristics in comparison to ribbed radiator. - Abstract: A kind of phase change material board (PCMB) was prepared for use in the thermal management of electronics, with paraffin and expanded graphite as the phase change material and matrix, respectively. The as-prepared PCMB presented a large thermal storage capacity of 141.74 J/g and enhanced thermal conductivity of 7.654 W/(m K). As a result, PCMB displayed much better cooling effect in comparison to natural air cooling, i.e., much lower heating rate and better uniformity of temperature distribution. On the other hand, compared with ribbed radiator technology, PCMB also presented different cooling characteristics, demonstrating that they were suitable for different practical application

  3. Preparation and thermal properties characterization of carbonate salt/carbon nanomaterial composite phase change material

    International Nuclear Information System (INIS)

    Tao, Y.B.; Lin, C.H.; He, Y.L.

    2015-01-01

    Highlights: • Nanocomposite phase change materials were prepared and characterized. • Larger specific surface area is more efficient to enhance specific heat. • Columnar structure is more efficient to enhance thermal conductivity. • Thermal conductivity enhancement is the key. • Single walled carbon nanotube is the optimal nanomaterial additive. - Abstract: To enhance the performance of high temperature salt phase change material, four kinds of carbon nanomaterials with different microstructures were mixed into binary carbonate eutectic salts to prepare carbonate salt/nanomaterial composite phase change material. The microstructures of the nanomaterial and composite phase change material were characterized by scanning electron microscope. The thermal properties such as melting point, melting enthalpy, specific heat, thermal conductivity and total thermal energy storage capacity were characterized. The results show that the nanomaterial microstructure has great effects on composite phase change material thermal properties. The sheet structure Graphene is the best additive to enhance specific heat, which could be enhanced up to 18.57%. The single walled carbon nanotube with columnar structure is the best additive to enhance thermal conductivity, which could be enhanced up to 56.98%. Melting point increases but melting enthalpy decreases with nanomaterial specific surface area increase. Although the additives decrease the melting enthalpy of composite phase change material, they also enhance the specific heat. As a combined result, the additives have little effects on thermal energy storage capacity. So, for phase change material performance enhancement, more emphasis should be placed on thermal conductivity enhancement and single walled carbon nanotube is the optimal nanomaterial additive

  4. Preparation of molybdenum borides by combustion synthesis involving solid-phase displacement reactions

    International Nuclear Information System (INIS)

    Yeh, C.L.; Hsu, W.S.

    2008-01-01

    Preparation of molybdenum borides of five different phases in the Mo-B binary system (including Mo 2 B, MoB, MoB 2 , Mo 2 B 5 , and MoB 4 ) was performed by self-propagating high-temperature synthesis (SHS) with two kinds of the reactant samples. When elemental powder compacts with an exact stoichiometry corresponding to the boride phase were employed, self-sustaining reaction was only achieved in the sample with Mo:B = 1:1 and nearly single-phase MoB was yielded. Therefore, the other four boride compounds were prepared from the reactant compacts composed of MoO 3 , Mo, and B powders, within which the displacement reaction of MoO 3 with boron was involved in combustion synthesis. Experimental evidence shows that the extent of displacement reaction in the overall reaction has a significant impact on sustainability of the synthesis reaction, combustion temperature, reaction front velocity, and composition of the end product. An increase in the solid-phase displacement reaction taking place during the SHS process contributes more heat flux to the synthesis reaction, thus resulting in the increase of combustion temperature and enhancement of the reaction front velocity. Based upon the XRD analysis, formation of Mo 2 B, MoB 2 , and Mo 2 B 5 as the dominant boride phase in the end product was successful through the SHS reaction with powder compacts under appropriate stoichiometries between MoO 3 , Mo, and B. However, a poor conversion was observed in the synthesis of MoB 4 . The powder compact prepared for the production of MoB 4 yielded mostly Mo 2 B 5

  5. Preparation of Phased and Merged Safety Analysis Reports for New DOE Nuclear Facilities

    International Nuclear Information System (INIS)

    BISHOP, G.E.

    2000-01-01

    The Spent Nuclear Fuels Project (SNFP) is charged with moving to storage 2,100 metric tons of spent nuclear fuel elements left over from plutonium production at DOE'S Hanford site in Washington state. Two new facilities, the Cold Vacuum Drying Facility (CVDF) and the Canister Storage Building (CSB) are in final construction. In order to meet aggressive schedule commitments, the SNFP chose to prepare the safety analysis reports (SAR's) in phases that covered only specific portions of each facility's design as it was built. Each SAR also merged the preliminary and final safety analysis reports into a single SAR, thereby covering all aspects of design, construction, and operation for that portion (phase) of the facility. A policy of ''NRC equivalency'' was also implemented in parallel with this effort, with the goal of achieving a rigor of safety analysis equivalent to that of NRC-licensed fuel processing facilities. DOE Order 5480.23. ''Nuclear Safety Analysis Reports'' allows preparation of both a phased and a merged SAR to accelerate construction schedules. However, project managers must be aware that such acceleration is not guaranteed. Managers considering this approach for their project should be cognizant of numerous obstacles that will be encountered. Merging and phasing SAR's will create new, unique, and unanticipated difficulties which may actually slow construction unless expeditiously and correctly managed. Pitfalls to be avoided and good practices to be implemented in preparing phased and merged SAR's are presented. The value of applying NRC requirements to the DOE safety analysis process is also discussed. As of December, 1999, the SNFP has completed and approved a SAR for the CVDF. Approval of the SAR for the CSB is pending

  6. Preparation and Characterization of TiB2-(Supra-Nano-Dual-Phase High-Entropy Alloy Cermet by Spark Plasma Sintering

    Directory of Open Access Journals (Sweden)

    Shulei Zhang

    2018-01-01

    Full Text Available This paper introduces the preparation method and characterization results of TiB2 ceramics with CoCrFeNiAl high-entropy alloy (HEA as a sintering aid by Spark Plasma Sintering (SPS. Good wettability between HEA and TiB2 was proved by the sessile drop method, indicating promising prospects for this composite. The sintering results showed that the addition of HEA could dramatically promote the sinterability of TiB2. TiB2-5 wt. % HEA dense ceramics prepared at the optimal temperature of 1650 °C showed fine morphology without formation of brittle phases. The liquid phase in the ceramics was highly consistent with the so-called “supra-nano-dual-phase materials (SNDPM”, with near-ideal strength. This study represents the first time that a ceramic-SNDPM composite has been fabricated since the invention of such structures.

  7. Preparation and Properties of Paraffin/TiO2/Active-carbon Composite Phase Change Materials

    Directory of Open Access Journals (Sweden)

    HAO Yong-gan

    2016-11-01

    Full Text Available A novel composite phase change materials (PCMs of paraffin/TiO2/active-carbon was prepared by a microemulsion method, where paraffin acted as a PCM and titanium dioxide (TiO2 as matrix material, and a small amount of active carbon was added to improve the thermal conductivity. The compositions, morphology and thermal properties of the paraffin/TiO2/active-carbon composite PCMs were characterized by XRD, SEM, TGA and DSC respectively. The shape stability during phase change process of this composite was also tested. The results show that paraffin is well encapsulated by TiO2 matrix, and thus exhibiting excellent shape-stabilized phase change feature. Besides, this composite PCM also presents superhydrophobic property. Therefore, these multifunctional features will endow PCMs with important application potential in energy efficient buildings.

  8. Preparation and performance of porous phase change polyethylene glycol/polyurethane membrane

    International Nuclear Information System (INIS)

    Ke Guizhen; Xie Huifang; Ruan Ruping; Yu Weidong

    2010-01-01

    Based on the theory of clotty porous phase change materials, the porous membrane was prepared with the blend of polyurethane (PU) and two polyethylene glycol (PEG) systems. Studied by scanning electron microscope (SEM), Fourier transform infrared (FT-IR), wide angle X-ray diffraction (WAXD), differential scanning calorimetry (DSC) and thermo-gravimetric (TG) tests, the morphology structure, chemical composition, crystalline morphology, phase change behaviors and thermal stability of porous phase change membrane were investigated. The results showed that the PU/PEG membrane had obvious porous structural feature, suitable transition temperature and high transition enthalpy. It is a flexible membrane with good energy storage function. When it is between solid and liquid transfer state in microcosms, the membrane can still keep solid shape in macroscopic state at high temperature during phase transition processing. It means that porous membrane PCM can be regarded as functional polymer. This method solved the problem of low working materials content in phase change textile. It succeeded in introducing the porous technology into functional textile's formation, and developed a new way to improve the phase change enthalpy largely for adjustable textile.

  9. An easily regenerable enzyme reactor prepared from polymerized high internal phase emulsions

    International Nuclear Information System (INIS)

    Ruan, Guihua; Wu, Zhenwei; Huang, Yipeng; Wei, Meiping; Su, Rihui; Du, Fuyou

    2016-01-01

    A large-scale high-efficient enzyme reactor based on polymerized high internal phase emulsion monolith (polyHIPE) was prepared. First, a porous cross-linked polyHIPE monolith was prepared by in-situ thermal polymerization of a high internal phase emulsion containing styrene, divinylbenzene and polyglutaraldehyde. The enzyme of TPCK-Trypsin was then immobilized on the monolithic polyHIPE. The performance of the resultant enzyme reactor was assessed according to the conversion ability of N_α-benzoyl-L-arginine ethyl ester to N_α-benzoyl-L-arginine, and the protein digestibility of bovine serum albumin (BSA) and cytochrome (Cyt-C). The results showed that the prepared enzyme reactor exhibited high enzyme immobilization efficiency and fast and easy-control protein digestibility. BSA and Cyt-C could be digested in 10 min with sequence coverage of 59% and 78%, respectively. The peptides and residual protein could be easily rinsed out from reactor and the reactor could be regenerated easily with 4 M HCl without any structure destruction. Properties of multiple interconnected chambers with good permeability, fast digestion facility and easily reproducibility indicated that the polyHIPE enzyme reactor was a good selector potentially applied in proteomics and catalysis areas. - Graphical abstract: Schematic illustration of preparation of hypercrosslinking polyHIPE immobilized enzyme reactor for on-column protein digestion. - Highlights: • A reactor was prepared and used for enzyme immobilization and continuous on-column protein digestion. • The new polyHIPE IMER was quite suit for protein digestion with good properties. • On-column digestion revealed that the IMER was easy regenerated by HCl without any structure destruction.

  10. An easily regenerable enzyme reactor prepared from polymerized high internal phase emulsions

    Energy Technology Data Exchange (ETDEWEB)

    Ruan, Guihua, E-mail: guihuaruan@hotmail.com [Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guangxi 541004 (China); Guangxi Collaborative Innovation Center for Water Pollution Control and Water Safety in Karst Area, Guilin University of Technology, Guilin 541004 (China); Wu, Zhenwei; Huang, Yipeng; Wei, Meiping; Su, Rihui [Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guangxi 541004 (China); Du, Fuyou, E-mail: dufu2005@126.com [Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guangxi 541004 (China); Guangxi Collaborative Innovation Center for Water Pollution Control and Water Safety in Karst Area, Guilin University of Technology, Guilin 541004 (China)

    2016-04-22

    A large-scale high-efficient enzyme reactor based on polymerized high internal phase emulsion monolith (polyHIPE) was prepared. First, a porous cross-linked polyHIPE monolith was prepared by in-situ thermal polymerization of a high internal phase emulsion containing styrene, divinylbenzene and polyglutaraldehyde. The enzyme of TPCK-Trypsin was then immobilized on the monolithic polyHIPE. The performance of the resultant enzyme reactor was assessed according to the conversion ability of N{sub α}-benzoyl-L-arginine ethyl ester to N{sub α}-benzoyl-L-arginine, and the protein digestibility of bovine serum albumin (BSA) and cytochrome (Cyt-C). The results showed that the prepared enzyme reactor exhibited high enzyme immobilization efficiency and fast and easy-control protein digestibility. BSA and Cyt-C could be digested in 10 min with sequence coverage of 59% and 78%, respectively. The peptides and residual protein could be easily rinsed out from reactor and the reactor could be regenerated easily with 4 M HCl without any structure destruction. Properties of multiple interconnected chambers with good permeability, fast digestion facility and easily reproducibility indicated that the polyHIPE enzyme reactor was a good selector potentially applied in proteomics and catalysis areas. - Graphical abstract: Schematic illustration of preparation of hypercrosslinking polyHIPE immobilized enzyme reactor for on-column protein digestion. - Highlights: • A reactor was prepared and used for enzyme immobilization and continuous on-column protein digestion. • The new polyHIPE IMER was quite suit for protein digestion with good properties. • On-column digestion revealed that the IMER was easy regenerated by HCl without any structure destruction.

  11. Preparation and characterization of macrocapsules containing microencapsulated PCMs (phase change materials) for thermal energy storage

    International Nuclear Information System (INIS)

    Han, Pengju; Lu, Lixin; Qiu, Xiaolin; Tang, Yali; Wang, Jun

    2015-01-01

    This paper was aimed to prepare, characterize and determine the comprehensive evaluation of promising composite macrocapsules containing microencapsulated PCMs (phase change materials) with calcium alginate gels as the matrix material. Macrocapsules containing microcapsules were fabricated by piercing-solidifying incuber method. Two kinds of microcapsules with n-tetradecane as core material, UF (urea-formaldehyde) and PMMA (poly(methyl methacrylate)) respectively as shell materials were prepared initially. For application concerns, thermal durability and mechanical property of macrocapsules were investigated by TGA (thermal gravimetric analysis) and Texture Analyser for the first time, respectively. The results showed excellent thermal stability and the compressive resistance of macrocapsules was sufficient for common application. The morphology and chemical structure of the prepared microcapsules and macrocapsules were characterized by SEM (scanning electron microscopy) and FT-IR (fourier transform infrared) spectroscopy method. Phase change behaviors and thermal durability of microcapsules and macrocapsules were investigated by DSC (differential scanning calorimetry). In order to improve latent heat of composite microcapsules, the core-shell weight ratio of tetradecane/UF shell microcapsules was chosen as 5.5:1 which obtained the phase change enthalpy of 194.1 J g −1 determined by DSC. In conclusion, these properties make it a feasible composite in applications of textile, building and cold-chain transportation. - Highlights: • We improved the phase change enthalpy with a higher core-shell ratio. • Urea-formaldehyde was firstly used as a shell material in the composite. • Mechanical and thermal durability property of the macrocapsules was firstly investigated in our work.

  12. Effect of applied voltage on phase components of composite coatings prepared by micro-arc oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Wenjun [Department of Prosthodontics, Guanghua School of Stomatology, Sun Yat-sen University, Guangzhou 510055 (China); Fang, Yu-Jing [Department of Colorectal Surgery, State Key Laboratory of Oncology in South China, Sun Yat-sen University Cancer Center, Guangzhou 510060 (China); Zheng, Huade [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Tan, Guoxin [Guangdong University of Technology, Guangdong Province 510006 (China); Cheng, Haimei [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China); Ning, Chengyun, E-mail: imcyning@scut.edu.cn [College of Materials Science and Engineering, South China University of Technology, Guangzhou 510641 (China)

    2013-10-01

    In this report, we present results from our experiments on composite coatings formed on biomedical titanium substrates by micro-arc oxidation (MAO) in constant-voltage mode. The coatings were prepared on the substrates in an aqueous electrolyte containing calcium acetate and β-glycerol phosphate disodium salt pentahydrate (β-GP). We analyzed the element distribution and phase components of the coatings prepared at different voltages by X-ray diffraction, thin-coating X-ray diffraction, electron-probe microanalysis, and Fourier-transform infrared spectroscopy. The results show that the composite coatings formed at 500 V consist of titania (TiO{sub 2}), hydroxylapatite (HA), and calcium carbonate (CaCO{sub 3}). Furthermore, the concentration of Ca, P, and Ti gradually changes with increasing applied voltage, and the phase components of the composite coatings gradually change from the bottom of the coating to the top: the bottom layer consists of TiO{sub 2}, the middle layer consists of TiO{sub 2} and HA, and the top layer consists of HA and a small amount of CaCO{sub 3}. The formation of HA directly on the coating surface by MAO technique can greatly enhance the surface bioactivity. - Highlights: • Coatings prepared on biomedical titanium substrate by micro-arc oxidation • Coatings composed of titania, hydroxyapatite and calcium carbonate • Hydroxyapatite on the coating surface can enhance the surface bioactivity.

  13. Biomimetic Silica Nanoparticles Prepared by a Combination of Solid-Phase Imprinting and Ostwald Ripening.

    Science.gov (United States)

    Piletska, Elena; Yawer, Heersh; Canfarotta, Francesco; Moczko, Ewa; Smolinska-Kempisty, Katarzyna; Piletsky, Stanislav S; Guerreiro, Antonio; Whitcombe, Michael J; Piletsky, Sergey A

    2017-09-14

    Herein we describe the preparation of molecularly imprinted silica nanoparticles by Ostwald ripening in the presence of molecular templates immobilised on glass beads (the solid-phase). To achieve this, a seed material (12 nm diameter silica nanoparticles) was incubated in phosphate buffer in the presence of the solid-phase. Phosphate ions act as a catalyst in the ripening process which is driven by differences in surface energy between particles of different size, leading to the preferential growth of larger particles. Material deposited in the vicinity of template molecules results in the formation of sol-gel molecular imprints after around 2 hours. Selective washing and elution allows the higher affinity nanoparticles to be isolated. Unlike other strategies commonly used to prepare imprinted silica nanoparticles this approach is extremely simple in nature and can be performed under physiological conditions, making it suitable for imprinting whole proteins and other biomacromolecules in their native conformations. We have demonstrated the generic nature of this method by preparing imprinted silica nanoparticles against targets of varying molecular mass (melamine, vancomycin and trypsin). Binding to the imprinted particles was demonstrated in an immunoassay (ELISA) format in buffer and complex media (milk or blood plasma) with sub-nM detection ability.

  14. Phase Composition of Samarium Niobate and Tantalate Thin Films Prepared by Sol-Gel Method

    Science.gov (United States)

    Bruncková, H.; Medvecký, Ľ.; Múdra, E.; Kovalčiková, A.; Ďurišin, J.; Šebek, M.; Girman, V.

    2017-12-01

    Samarium niobate SmNbO4 (SNO) and tantalate SmTaO4 (STO) thin films ( 100 nm) were prepared by sol-gel/spin-coating process on alumina substrates with PZT interlayer and annealing at 1000°C. The precursors of films were synthesized using Nb or Ta tartrate complexes. The improvement of the crystallinity of monoclinic M'-SmTaO4 phase via heating was observed through the coexistence of small amounts of tetragonal T-SmTa7O19 phase in STO precursor at 1000°C. The XRD results of SNO and STO films confirmed monoclinic M-SmNbO4 and M'-SmTaO4 phases, respectively, with traces of orthorhombic O-SmNbO4 (in SNO). In STO film, the single monoclinic M'-SmTaO4 phase was revealed. The surface morphology and topography of thin films were investigated by SEM and AFM analysis. STO film was smoother with roughness 3.2 nm in comparison with SNO (6.3 nm). In the microstructure of SNO film, small spherical ( 50 nm) and larger cuboidal particles ( 100 nm) of the SmNbO4 phase were observed. In STO, compact clusters composed of fine spherical SmTaO4 particles ( 20-50 nm) were found. Effect of samarium can contribute to the formation different polymorphs of these films for the application to environmental electrolytic thin film devices.

  15. UV irradiation-initiated MMA polymerization to prepare microcapsules containing phase change paraffin

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Sude; Song, Guolin; Li, Wei; Fan, Pengfei; Tang, Guoyi [Institute of Advanced Materials, Graduated School at Shenzhen, Tsinghua University, Shenzhen 518055 (China)

    2010-10-15

    Microencapsulated phase change material (MEPCM), paraffin, with polymethylmethacrylate shell was prepared by introducing UV irradiation to an O/W emulsion polymerization for approximately 30 min under constant stirring. The results of differential scanning calorimetry analyses indicate that the latent heat and the content of paraffin of microcapsules are 101 J g{sup -1} and 61.2 wt%, respectively. The phase transition temperature of MEPCM ranges from 24 to 33 C. The MEPCM was characterized using scanning electron microscopy and Fourier transform infrared spectroscopy. Thermal gravimetric analysis results show that the MEPCM is degraded into two distinguishable steps. Accelerated thermal cycling tests also indicate that the MEPCM displays a good thermal reliability. Gypsum boards composed of as-prepared MEPCM show a good temperature-regulated property. Based on all these results, it can be concluded that the microencapsulated paraffin as MEPCMs have good potential for thermal energy storage purposes such as phase change material slurries, solar space heating applications, textiles and building materials. (author)

  16. Preparation and initial characterization of fluidized bed steam reforming pure-phase standards

    Energy Technology Data Exchange (ETDEWEB)

    Missimer, D. M.; Rutherford, R. L.

    2013-03-21

    Hanford is investigating the Fluidized Bed Steam Reforming (FBSR) process for their Low Activity Waste. The FBSR process offers a low-temperature continuous method by which liquid waste can be processed with the addition of clay into a sodium aluminosilicate (NAS) waste form. The NAS waste form is mainly comprised of nepheline (NaAlSiO{sub 4}), sodalite (Na{sub 8}[AlSiO{sub 4}]{sub 6}Cl{sub 2}), and nosean (Na{sub 8}[AlSiO{sub 4}]{sub 6}SO{sub 4}). Anions such as perrhenate (ReO{sub 4}{sup -}), pertechnetate (TcO{sub 4}{sup -}), and iodine (I{sup -}) are expected to replace sulfate in the nosean structure and/or chloride in the sodalite mineral structure (atomically bonded inside the aluminosilicate cages that these mineral structures possess). In the FBSR waste form, each of these phases can exist in a variety of solid solutions that differ from the idealized forms observed in single crystals in nature. The lack of understanding of the durability of these stoichiometric or idealized mineral phases complicates the ability to deconvolute the durability of the mixed phase FBSR product since it is a combination of different NAS phases. To better understand the behavior, fabrication and testing of the individual phases of the FBSR product is required. Analytical Development (AD) of the Science and Technology directorate of the Savannah River National Laboratory (SRNL) was requested to prepare the series of phase-pure standards, consisting of nepheline, nosean, and Cl, Re, and I sodalite. Once prepared, X-ray Diffraction (XRD) analyses were used to confirm the products were phase pure. These standards are being used for subsequent characterization studies consisting of the following: single-pass flow-through (SPFT) testing, development of thermodynamic data, and x-ray diffraction (XRD) calibration curves. In addition to the above mentioned phase-pure standards, AD was tasked with fabricating a mixed Tc-Re sodalite.

  17. A FTIR study water in membrane of nitrocellulose prepared by phase inversion

    International Nuclear Information System (INIS)

    Benosmane, N.; Boutemeur, B.; Hamdi, M.

    2004-01-01

    Full text.Cellulose derivates were the first biopolymers used to produce synthesis membranes for technical applications, in this study the state of water in asymmetric membrane of nitrocellulose, prepared by the phase inversion process, was investigated using infrared spectroscopy (FTIR), after membrane preparation by the wet inversion process in acetone, the spectre FTIR of wet asymmetric membrane of nitrocellulose after immersion in water (after one week) is compared to the spectre of dried asymmetric membrane of nitrocellulose, the difference in spectre of dried and wet membrane indicate a weakly hydrogen-bonded to the polymer hydroxyl groups between water and hydroxyl groups in surface of membrane, the results demonstrate the amount of water species present in the surface of asymmetric membrane and heterogeneous of surface

  18. Process for preparation of a solid-phase radioimmunoassay support and use thereof

    International Nuclear Information System (INIS)

    Meriadec, B.; Roubertie, P.

    1979-01-01

    A process is described for the preparation of a support useful in radioimmunoassay chromatographic columns. The process involves the preparation of a chromatographic gel capable of selectively retaining one or more components contained in an antigen-antibody-containing solution. The gel is bound to the appropriate antiserum, then freeze-dried, pulverized and compressed into a tablet. The tablet support swells upon contact with an antigen-antibody-containing solution to conform to the shape of the columns. An example of the application of this support in the radioimmunoassay of thyroid-stimulating hormone is described. This type of support is also particularly useful in second antibody solid phase radioimmunoassays since there is no limit to the size of the antigen to which this technology may be applied. (U.K.)

  19. Purification of flavonoids from licorice using an off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method.

    Science.gov (United States)

    Fan, Yunpeng; Fu, Yanhui; Fu, Qing; Cai, Jianfeng; Xin, Huaxia; Dai, Mei; Jin, Yu

    2016-07-01

    An orthogonal (71.9%) off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method coupled with effective sample pretreatment was developed for separation and purification of flavonoids from licorice. Most of the nonflavonoids were firstly removed using a self-made Click TE-Cys (60 μm) solid-phase extraction. In the first dimension, an industrial grade preparative chromatography was employed to purify the crude flavonoids. Click TE-Cys (10 μm) was selected as the stationary phase that provided an excellent separation with high reproducibility. Ethyl acetate/ethanol was selected as the mobile phase owing to their excellent solubility for flavonoids. Flavonoids co-eluted in the first dimension were selected for further purification using reversed-phase liquid chromatography. Multiple compounds could be isolated from one normal-phase fraction and some compounds with bad resolution in one-dimensional liquid chromatography could be prepared in this two-dimensional system owing to the orthogonal separation. Moreover, this two-dimensional liquid chromatography method was beneficial for the preparation of relatively trace flavonoid compounds, which were enriched in the first dimension and further purified in the second dimension. Totally, 24 flavonoid compounds with high purity were obtained. The results demonstrated that the off-line two-dimensional liquid chromatography method was effective for the preparative separation and purification of flavonoids from licorice. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Preparation and Thermal Properties of Eutectic Hydrate Salt Phase Change Thermal Energy Storage Material

    OpenAIRE

    Liang, Lin; Chen, Xi

    2018-01-01

    In this study, a new cold storage phase change material eutectic hydrate salt (K2HPO4·3H2O–NaH2PO4·2H2O–Na2S2O3·5H2O) was prepared, modified, and tested. The modification was performed by adding a nucleating agent and thickener. The physical properties such as viscosity, surface tension, cold storage characteristics, supercooling, and the stability during freeze-thaw cycles were studied. Results show that the use of nucleating agents, such as sodium tetraborate, sodium fluoride, and nanoparti...

  1. Implementation of quantum controlled phase gate and preparation of multiparticle entanglement in cavity QED

    International Nuclear Information System (INIS)

    Wu Xi; Chen Zhi-Hua; Chen Yue-Hua; Ye Ming-Yong; Lin Xiu-Min; Zhang Yong

    2011-01-01

    Schemes are presented for realizing quantum controlled phase gate and preparing an N-qubit W-like state, which are based on the large-detuned interaction among three-state atoms, dual-mode cavity and a classical pulse. In particular, a class of W states that can be used for perfect teleportation and superdense coding is generated by only one step. Compared with the previous schemes, cavity decay is largely suppressed because the cavity is only virtually excited and always in the vacuum state and the atomic spontaneous emission is strongly restrained due to a large atom—field detuning. (general)

  2. Enhanced field emission from PbTiO{sub 3} nanodots prepared by phase separation approach

    Energy Technology Data Exchange (ETDEWEB)

    Li Jinna; Luo Ming [Department of Materials Science and Engineering, State Key Laboratory of Silicon Materials, Zhejiang University, Hangzhou 310027 (China); Weng Wenjian, E-mail: wengwj@zju.edu.cn [Department of Materials Science and Engineering, State Key Laboratory of Silicon Materials, Zhejiang University, Hangzhou 310027 (China); Cheng Kui; Du Piyi; Shen Ge; Han Gaorong [Department of Materials Science and Engineering, State Key Laboratory of Silicon Materials, Zhejiang University, Hangzhou 310027 (China)

    2009-10-15

    Uniformly distributed PbTiO{sub 3} nanodots were successfully prepared by phase separation approach. A precursor sol film was first spin-coated on Si wafer and then spontaneously separated into two distinct phases owing to the Marangoni instability. PT nanodots with tailorable size and density were obtained after further heat treatment. X-ray diffraction analysis indicated that these nanodots showed a perovskite structure. An excellent room temperature field emission property of PbTiO{sub 3} nanodots was observed: the minimum turn-on voltage was about 5.3 V/{mu}m; while the emission current density reached about 270 {mu}A cm{sup -2} at an applied field of about 9.25 V/{mu}m.

  3. Preparation of bioconjugates by solid-phase conjugation to ion exchange matrix-adsorbed carrier proteins

    DEFF Research Database (Denmark)

    Houen, G.; Olsen, D.T.; Hansen, P.R.

    2003-01-01

    A solid-phase conjugation method utilizing carrier protein bound to an ion exchange matrix was developed. Ovalbumin was adsorbed to an anion exchange matrix using a batch procedure, and the immobilized protein was then derivatized with iodoacetic acid N-hydroxysuccinimid ester. The activated......, and immunization experiments with the eluted conjugates showed that the more substituted conjugates gave rise to the highest titers of glutathione antibodies. Direct immunization with the conjugates adsorbed to the ion exchange matrix was possible and gave rise to high titers of glutathione antibodies. Conjugates...... of ovalbumin and various peptides were prepared in a similar manner and used for production of peptide antisera by direct immunization with the conjugates bound to the ion exchanger. Advantages of the method are its solid-phase nature, allowing fast and efficient reactions and intermediate washings...

  4. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

    International Nuclear Information System (INIS)

    Luo Fan; Wu Zucheng; Tao Ping; Cong Yanqing

    2009-01-01

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 μg L -1 , the linear ranges were between 0.6 and 35619 μg L -1 with good linearity (R 2 = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds

  5. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction.

    Science.gov (United States)

    Luo, Fan; Wu, Zucheng; Tao, Ping; Cong, Yanqing

    2009-01-05

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 microg L(-1), the linear ranges were between 0.6 and 35,619 microg L(-1) with good linearity (R(2)=0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

  6. Preparation and thermal properties of short carbon fibers/erythritol phase change materials

    International Nuclear Information System (INIS)

    Zhang, Qiang; Luo, Zhiling; Guo, Qilin; Wu, Gaohui

    2017-01-01

    Highlights: • Short carbon fiber (SCF)/erythritol phase change composites (PCCs) are prepared and tested. • The PCCs possess large heat capacity and high thermal conductivity. • The size of SCFs can affect thermal conductivities of SCF/erythritol PCCs. • The size of SCFs has negligible effects on melting points and enthalpies. • The SCF/erythritol PCCs show good temperature-regulated property. - Abstract: The thermal properties of the short carbon fibers (SCFs) filled erythritol phase change composites (PCCs) were investigated experimentally. The samples were prepared with different mass loadings of two kinds of SCFs, 1%, 2%, 4%, 7% and 10%. The melting points and phase change enthalpies were measured by differential scanning calorimeter (DSC). The effects of SCFs on the melting points are relatively small but the enthalpies were reduced with the loadings of SCFs. The greatest loss of enthalpies is 11.3% for composites filled with 10% SCFs. The thermal conductivities increased with the loadings of SCFs but not linearly. The highest thermal conductivity is 3.92 W/(m⋅K) for the composites with 10% longer SCFs, which was enhanced by 407.8% compared to pure erythritol (0.77 W/(m⋅K)). Composites filled with longer SCFs possess higher thermal conductivity and the mechanisms were discussed. A simple setup was made to test the temperature-regulated property of these materials. These include pure erythritol and phase change composites with different loading of SCFs. The PCCs have shown good application potential and the longer SCFs can lead to the better performance of PCCs.

  7. [Preparation and performance characterization of gold nanoparticles modified chiral capillary electrochromatography stationary phase].

    Science.gov (United States)

    Xiong, Lele; Li, Ruijun; Ji, Yibing

    2017-07-08

    Gold nanoparticles (GNPs, 15 nm) were prepared and introduced to amino groups derived silica monolithic column. Bovine serum albumin (BSA) was immobilized via covalent modification method onto the carboxylic functionalized GNPs to afford chiral stationary phase (CSP) for enantioseparation. GNPs were well dispersed and successfully incorporated onto the columns with the contents as high as 17.18% by characterization method such as transmission electron microscopy (TEM), ultraviolet (UV)-visible absorption spectra and scanning electron microscopy (SEM). The preparation conditions of the BSA modified CSP were optimized and 10% (v/v) 3-aminopropyltriethoxysilane (APTES) and 15 g/L BSA were selected as appropriate reaction conditions. The enantioseparation performance of the BSA modified CSP has been investigated by capillary electrochromatography (CEC). Enantiomers of tryptophan, ephedrine and atenolol were resolved, and the baseline separation of tryptophan was achieved. Meanwhile, the influences of pH value, buffer concentrations and applied voltages used on the chiral separation were studied, and the optimal separation conditions were 10 mmol/L phosphate buffer at pH 7.4 and 15 kV applied voltages. In comparison with the BSA modified CSP prepared by physical adsorption, the CSP prepared by covalent modification method had better separation results, and the analytes could be separated directly without pre-column derivatization. In addition, the prepared BSA modified CSP exhibited good run to run repeatability with relative standard deviations (RSDs) of the migration times and selectivity factors not more than 2.3% and 0.96%, respectively. This work offers a good thinking for modification with other proteins or other types of chiral selectors.

  8. Preparation of CMC-modified melamine resin spherical nano-phase change energy storage materials.

    Science.gov (United States)

    Hu, Xiaofeng; Huang, Zhanhua; Zhang, Yanhua

    2014-01-30

    A novel carboxymethyl cellulose (CMC)-modified melamine-formaldehyde (MF) phase change capsule with excellent encapsulation was prepared by in situ polymerization. Effects of CMC on the properties of the capsules were studied by Fourier transformation infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), scanning electronic microscopy (SEM), X-ray diffractometry (XRD), and thermogravimetric analysis (TGA). The results showed that the CMC-modified capsules had an average diameter of about 50nm and good uniformity. The phase change enthalpy of the capsules was increased and the cracking ratio decreased by incorporating a suitable amount of CMC. The optimum phase change enthalpy of the nanocapsules was 83.46J/g, and their paraffin content was 63.1%. The heat resistance of the capsule shells decreased after CMC modification. In addition, the nanocapsule cracking ratio of the nanocapsules was 11.0%, which is highly attractive for their application as nano phase change materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. Current Status of HCCR TBM Design for the Preliminary Design Phase Preparation

    Energy Technology Data Exchange (ETDEWEB)

    Park, Seong Dae; Lee, Dong Won; Kim, Dong Jun [KAERI, Daejeon (Korea, Republic of); Ahn, Mu Young [NFRI, Daejeon (Korea, Republic of)

    2016-05-15

    Helium cooled ceramic reflector (HCCR) TBM-set will be installed in the equatorial port no.18 of ITER inside the vacuum vessel directly facing the plasma. TBM-set refers the TBM and associated shield and connecting support. After the Conceptual Design Review (CDR), Helium Cooled Ceramic Reflector (HCCR) Test Blanket Module (TBM) design is being updated for the preparation of the preliminary design phase. The manufacturability is considered based on the TBM-set model of the conceptual design phase. In this work, the design changes for each component of the TBM-set is described in comparison with the CD phase. The current design direction and details is presented. The first wall (FW) is component facing the plasma directly. This component should have a superior cooling performance. Present Helium Cooled Ceramic Reflector (HCCR) Test Blanket Module (TBM) design was described in comparison with the CD model. The manufacturability was considered in current PD phase. The detained design of the connecting support will be determined reflecting the load assessment. The structural integrity will be confirmed with a various load condition.

  10. Preparation of gold microparticles using halide ions in bulk block copolymer phases via photoreduction

    International Nuclear Information System (INIS)

    Cha, Sang-Ho; Kim, Ki-Hyun; Lee, Won-Ki; Lee, Jong-Chan

    2009-01-01

    Gold microparticles were prepared from the gold salt in the solid bulk phase of a poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) block copolymer via a photoreduction process in the presence of halide ions. The shapes and sizes of the gold microparticles were found to be dependent on the types and amount of halide ions as well as the types of cations used due to the combined effects of the adsorption power and oxidative dissolution ability of the additives on gold surfaces. Gold nanorods were obtained when poly(ethylene oxide) was used instead of the block copolymer. This suggests that the poly(propylene oxide) (PPO) parts in the block copolymer are essential for the formation of gold microparticles, even though the degree of the direct interaction between the PPO blocks and gold salt is not significant. - Graphical abstract: Gold microparticles were successfully prepared using halide ions as additives in the polymeric bulk phase via photoreduction with the glow lamp irradiation.

  11. Methodology transfer for the preparation of NPP decommissioning for leading personnel of the Ignalina NPP and for the representatives of Lithuanian authorities

    International Nuclear Information System (INIS)

    Ackermann, L.; Baecker, A.

    2004-01-01

    At request of the Lithuanian government to receive support for the preparation of the decommissioning of Ignalina NPP, a bilateral project was financed by the German federal government to transfer experience from the decommissioning of the Greifswald and Rheinsberg NPPs to the management staff of the Ignalina NPP and to the representatives of the Lithuanian authorities in charge of the decommissioning. The methodology transfer project was prepared and carried out under the leadership of the Gesellschaft fuer Anlagen- und Reaktorsicherheit (GRS) mbH. The practical implementation was within the responsibility of Energiewerke Nord GmbH (EWN) in cooperation with other German subcontractors. The methodology transfer comprised the task fields of project management, project planning, licensing procedure and waste management as well as social aspects of the further development of the industrial site. Five intensive one-week seminars were conducted mainly at the Greifswald NPP site and the knowledge gained was then consolidated in two evaluation seminars at the Ignalina NPP. As the basis for the training realised in 2002 and 2003, EWN provided about 2000 power-point illustrations, more than 200 transparencies and four video films. The training handouts produced by EWN were delivered to the seminar participants in Russian and English language and documented in the database ''Technische Dokumentation Ost'' (DOKU OST) of GRS. (orig.)

  12. Preparation and thermal energy storage properties of paraffin/expanded graphite composite phase change material

    International Nuclear Information System (INIS)

    Zhang, Zhengguo; Zhang, Ni; Peng, Jing; Fang, Xiaoming; Gao, Xuenong; Fang, Yutang

    2012-01-01

    Highlights: ► EG was obtained by microwave irradiation to prepare the paraffin/EG composite PCM. ► Composite PCM was characterized by XRD to investigate the chemical compatibility. ► Temperature profiles of the composite PCM were obtained during thermal energy storage. -- Abstract: The paraffin/expanded graphite (EG) composite phase change material (PCM) was prepared by absorbing liquid paraffin into EG, in which paraffin was chosen as the PCM. EG was produced by microwave irradiation performed at room temperature. It was found that the EG prepared at 800 W irradiation power for 10 s exhibited the maximum sorption capacity of 92 wt% for paraffin. Scanning electron microscopy images showed that paraffin was uniformly dispersed in the pores of EG. Differential scanning calorimeter analysis indicated that the melting temperature of the composite PCM was close to that of paraffin, and its latent heat was equivalent to the calculated value based on the mass fraction of paraffin in the composite. X-ray diffraction analysis showed that the composite PCM was just a combination of paraffin with EG, and no new substance was produced. Thermal energy storage performance of the composite PCM was tested in a latent thermal energy storage (LTES) system. Transients of axial and radial temperature profiles were obtained in the LTES for the composite PCM and paraffin. The thermal energy storage charging duration for the composite PCM was reduced obviously compared to paraffin.

  13. Modern Evaluation of Liquisolid Systems with Varying Amounts of Liquid Phase Prepared Using Two Different Methods

    Directory of Open Access Journals (Sweden)

    Barbora Vraníková

    2015-01-01

    Full Text Available Liquisolid systems are an innovative dosage form used for enhancing dissolution rate and improving in vivo bioavailability of poorly soluble drugs. These formulations require specific evaluation methods for their quality assurance (e.g., evaluation of angle of slide, contact angle, or water absorption ratio. The presented study is focused on the preparation, modern in vitro testing, and evaluation of differences of liquisolid systems containing varying amounts of a drug in liquid state (polyethylene glycol 400 solution of rosuvastatin in relation to an aluminometasilicate carrier (Neusilin US2. Liquisolid powders used for the formulation of final tablets were prepared using two different methods: simple blending and spraying of drug solution onto a carrier in fluid bed equipment. The obtained results imply that the amount of liquid phase in relation to carrier material had an effect on the hardness, friability, and disintegration of tablets, as well as their height. The use of spraying technique enhanced flow properties of the prepared mixtures, increased hardness values, decreased friability, and improved homogeneity of the final dosage form.

  14. Preparation of Biofuel from Palm Oil Catalyzed by Ammonium Molybdate in Homogeneous Phase

    Directory of Open Access Journals (Sweden)

    Sepehr Sadighi

    2017-04-01

    Full Text Available Producing transportation fuels from bio sources was of prime importance due to the strict environmental legislations for producing clean fuels from conventional oil resources. However, the economical impacts of the biofuel production should be considered. In this study, the production of bio-naphtha and biodiesel from palm oil using homogeneous catalyst, i.e. an aqueous phase of ammonium molybdate, was studied. This catalyst was prepared by dissolving sodium molybdate in de-ionized water with hydrochloric acid, and then neutralizing the mixture with ammonium hydroxide. The solution was dried at 90 °C for 24 h to obtain ammonium molybdate. Then, characterization of the catalyst was done by informative techniques, such as XRD and FT-IR. The results showed that the main phase of the synthesized catalyst was molybdate ammonium hydrates (4MoO3.2NH3.H2O, and also bands of Mo–O, Mo–O–Mo, N–H and surface hydroxyl groups were observed in the sample. Moreover, activity test confirms that the bio-naphtha produced from the proposed method has a few aromatic components, and its sulfur content was negligible. Moreover, ash, nitrogen, sulfur and carbon residue were not detected in the produced biodiesel, and its Cetane index was 66.3. Therefore, it was a suitable fuel for diesel engines vehicles. Copyright © 2017 BCREC GROUP. All rights reserved Received: 3rd May 2016; Revised: 1st October 2016; Accepted: 18th October 2016 How to Cite: Sadighi, S., Targhi, S.K.M. (2017. Preparation of Biofuel from Palm Oil Catalyzed by Ammonium Molybdate in Homogeneous Phase. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (1: 49-54 (doi:10.9767/bcrec.12.1.486.49-54 Permalink/DOI: http://dx.doi.org/10.9767/bcrec.12.1.486.49-54

  15. Phase transition of Ni-Mn-Ga alloy powders prepared by vibration ball milling

    International Nuclear Information System (INIS)

    Tian, B.; Chen, F.; Tong, Y.X.; Li, L.; Zheng, Y.F.; Liu, Y.; Li, Q.Z.

    2011-01-01

    Research highlights: → The vibration ball milling with a high milling energy introduces the atomic disorder and large lattice distortion in the alloy during milling and makes the formation of disordered fcc structure phase in the alloy. → The transition temperature and activation energy for disordered fcc → disordered bcc are ∼320 o C and 209 ± 8 kJ/mol, respectively. → The alloy powders annealed at 800 o C for 1 h show a one-stage martensitic transformation with quite lower latent heat compared to the bulk alloy. - Abstract: This study investigated the phase transformation of the flaky shaped Ni-Mn-Ga powder particles with thickness around 1 μm prepared by vibration ball milling and post-annealing. The SEM, XRD, DSC and ac magnetic susceptibility measurement techniques were used to characterize the Ni-Mn-Ga powders. The structural transition of Heusler → disordered fcc occurred in the powders prepared by vibration ball milling (high milling energy) for 4 h, which was different from the structural transition of Heusler → disordered fct of the powders fabricated by planetary ball milling (low milling energy) for 4 h. The two different structures after ball milling should be due to the larger lattice distortion occurred in the vibration ball milling process than in the planetary ball milling process. The structural transition of disordered fcc → disordered bcc took place at ∼320 o C during heating the as-milled Ni-Mn-Ga powders, which was attributed to the elimination of lattice distortion caused by ball milling. The activation energy for this transition was 209 ± 8 kJ/mol. The Ni-Mn-Ga powder annealed at 800 o C mainly contained Heusler austenite phase at room temperature and showed a low volume of martensitic transformation upon cooling. The inhibition of martensitic transformation might be attributed to the reduction of grain size in the annealed Ni-Mn-Ga particles.

  16. Nanocellulose Derivative/Silica Hybrid Core-Shell Chiral Stationary Phase: Preparation and Enantioseparation Performance

    Directory of Open Access Journals (Sweden)

    Xiaoli Zhang

    2016-05-01

    Full Text Available Core-shell silica microspheres with a nanocellulose derivative in the hybrid shell were successfully prepared as a chiral stationary phase by a layer-by-layer self-assembly method. The hybrid shell assembled on the silica core was formed using a surfactant as template by the copolymerization reaction of tetraethyl orthosilicate and the nanocellulose derivative bearing triethoxysilyl and 3,5-dimethylphenyl groups. The resulting nanocellulose hybrid core-shell chiral packing materials (CPMs were characterized and packed into columns, and their enantioseparation performance was evaluated by high performance liquid chromatography. The results showed that CPMs exhibited uniform surface morphology and core-shell structures. Various types of chiral compounds were efficiently separated under normal and reversed phase mode. Moreover, chloroform and tetrahydrofuran as mobile phase additives could obviously improve the resolution during the chiral separation processes. CPMs still have good chiral separation property when eluted with solvent systems with a high content of tetrahydrofuran and chloroform, which proved the high solvent resistance of this new material.

  17. Phase transitions of sodium niobate powder and ceramics, prepared by solid state synthesis

    Science.gov (United States)

    Koruza, J.; Tellier, J.; Malič, B.; Bobnar, V.; Kosec, M.

    2010-12-01

    Phase transitions of sodium niobate, prepared by the solid state synthesis method, were examined using dielectric measurements, differential scanning calorimetry, and high temperature x-ray diffraction, in order to contribute to the clarification of its structural behavior below 400 °C. Four phase transitions were detected in the ceramic sample using dielectric measurements and differential scanning calorimetry and the obtained temperatures were in a good agreement with previous reports for the transitions of the P polymorph. The anomaly observed by dielectric measurements in the vicinity of 150 °C was frequency dependent and could be related to the dynamics of the ferroelectric nanoregions. The phase transitions of the as-synthesized NaNbO3 powder were investigated using differential scanning calorimetry and high temperature x-ray diffraction. The results show the existence of the Q polymorph at room temperature, not previously reported for the powder, which undergoes a transition to the R polymorph upon heating through a temperature region between 265 and 326.5 °C. This transition is mainly related to the displacement of Na into a more symmetric position and a minor change in the tilting system. The structures at room temperature, 250, 300, and 420 °C were refined by the Rietveld method and the evolution of the tilting system of the octahedral network and cationic displacement are reported.

  18. Phase transitions of sodium niobate powder and ceramics, prepared by solid state synthesis

    International Nuclear Information System (INIS)

    Koruza, J.; Tellier, J.; Malic, B.; Bobnar, V.; Kosec, M.

    2010-01-01

    Phase transitions of sodium niobate, prepared by the solid state synthesis method, were examined using dielectric measurements, differential scanning calorimetry, and high temperature x-ray diffraction, in order to contribute to the clarification of its structural behavior below 400 deg. C. Four phase transitions were detected in the ceramic sample using dielectric measurements and differential scanning calorimetry and the obtained temperatures were in a good agreement with previous reports for the transitions of the P polymorph. The anomaly observed by dielectric measurements in the vicinity of 150 deg. C was frequency dependent and could be related to the dynamics of the ferroelectric nanoregions. The phase transitions of the as-synthesized NaNbO 3 powder were investigated using differential scanning calorimetry and high temperature x-ray diffraction. The results show the existence of the Q polymorph at room temperature, not previously reported for the powder, which undergoes a transition to the R polymorph upon heating through a temperature region between 265 and 326.5 deg. C. This transition is mainly related to the displacement of Na into a more symmetric position and a minor change in the tilting system. The structures at room temperature, 250, 300, and 420 deg. C were refined by the Rietveld method and the evolution of the tilting system of the octahedral network and cationic displacement are reported.

  19. Hole-expansion formability of dual-phase steels using representative volume element approach with boundary-smoothing technique

    International Nuclear Information System (INIS)

    Kim, Ji Hoon; Lee, M.G.; Kim, D.; Matlock, D.K.; Wagoner, R.H.

    2010-01-01

    Research highlights: → Robust microstructure-based FE mesh generation technique was developed. → Local deformation behavior near phase boundaries could be quantitatively understood. → Macroscopic failure could be connected to microscopic deformation behavior of multi-phase steel. - Abstract: A qualitative analysis was carried out on the formability of dual-phase (DP) steels by introducing a realistic microstructure-based finite element approach. The present microstructure-based model was constructed using a mesh generation process with a boundary-smoothing algorithm after proper image processing. The developed model was applied to hole-expansion formability tests for DP steel sheets having different volume fractions and morphological features. On the basis of the microstructural inhomogeneity observed in the scanning electron micrographs of the DP steel sheets, it was inferred that the localized plastic deformation in the ferritic phase might be closely related to the macroscopic formability of DP steel. The experimentally observed difference between the hole-expansion formability of two different microstructures was reasonably explained by using the present finite element model.

  20. "Chromoseratops Meiosus": A Simple, Two-Phase Exercise to Represent the Connection between Meiosis & Increased Genetic Diversity

    Science.gov (United States)

    Eliyahu, Dorit

    2014-01-01

    I present an activity to help students make the connection between meiosis and genetic variation. The students model meiosis in the first phase of the activity, and by that process they produce gametes of a fictitious reptilobird species, "Chromoseratops meiosus." Later on, they will "mate" their gametes and produce a zygote…

  1. Preparation of meta-stable phases of barium titanate by Sol-hydrothermal method

    Directory of Open Access Journals (Sweden)

    Mahalakshmi Selvaraj

    2015-11-01

    Full Text Available Two low-cost chemical methods of sol–gel and the hydrothermal process have been strategically combined to fabricate barium titanate (BaTiO3 nanopowders. This method was tested for various synthesis temperatures (100 °C to 250 °C employing barium dichloride (BaCl2 and titanium tetrachloride (TiCl4 as precursors and sodium hydroxide (NaOH as mineralizer for synthesis of BaTiO3 nanopowders. The as-prepared BaTiO3 powders were investigated for structural characteristics using x-ray diffraction (XRD, scanning electron microscopy (SEM and transmission electron microscopy (TEM. The overall analysis indicates that the hydrothermal conditions create a gentle environment to promote the formation of crystalline phase directly from amorphous phase at the very low processing temperatures investigated. XRD analysis showed phase transitions from cubic - tetragonal - orthorhombic - rhombohedral with increasing synthesis temperature and calculated grain sizes were 34 – 38 nm (using the Scherrer formula. SEM and TEM analysis verified that the BaTiO3 nanopowders synthesized by this method were spherical in shape and about 114 - 170 nm in size. The particle distribution in both SEM and TEM shows that as the reaction temperature increases from 100 °C to 250 °C, the particles agglomerate. Selective area electron diffraction (SAED shows that the particles are crystalline in nature. The study shows that choosing suitable precursor and optimizing pressure and temperature; different meta-stable (ferroelectric phases of undoped BaTiO3 nanopowders can be stabilized by the sol-hydrothermal method.

  2. The first preparative solution phase synthesis of melanotan II

    Directory of Open Access Journals (Sweden)

    2008-10-01

    Full Text Available Melanotan II is a synthetic cyclic heptapeptide used to prevent a sunlight-induced skin cancer by stimulating the skin tanning process. In this paper we report the first solution phase synthesis of the title compound. The hexapeptide sequence has been assembled by [(2+2+1+1] scheme. After removing the orthogonal protection, a carbodiimide mediated lactamization, involving the ε-amino group of lysine and γ-carboxy group of aspartic acid, led to a cyclic intermediate. Appending N-acetylnorleucine concluded the assembly of melanotan II molecule. Protection of the lateral groups in arginine and tryptophan was omitted for atom and step economy reasons. The total synthesis of melanotan II was accomplished in 12 steps with 2.6% overall yield, affording >90% pure peptide without using preparative chromatography.

  3. Composite phase change materials prepared by encapsuling paraffin in PVC macrocapsules

    International Nuclear Information System (INIS)

    Chen, Yingbo; Zhang, Shifeng; Zhang, Qi; Chen, Yusheng; Zhang, Yufeng

    2014-01-01

    Highlights: • PVC macrocapsules coated with SiO 2 were synthesized. • Paraffin was encapsuled in the capsules. • The composite PCM has high heat capacity. • The composite PCM has no surpercooling. - Abstract: A novel phase change material capsules with SiO 2 in their surface was prepared by absorbing paraffin into PVC hollow capsules and by the polycondensation reaction of TEOS in different conditions. X-ray photoelectron spectroscopy (XPS) analysis and scanning electronic microscope (SEM) were used to determine chemical composition and microstructure of the composite capsules, respectively. Enthalpy capacity and thermal stability of the composite capsules are systematically characterized by using differential scanning calorimeter (DSC), thermogravimetric analyzer (TGA) and thermocycling tests. The composite has high heat capacity with good stability and absence of supercooling phenomena

  4. Sodium ion conducting polymer electrolyte membrane prepared by phase inversion technique

    Science.gov (United States)

    Harshlata, Mishra, Kuldeep; Rai, D. K.

    2018-04-01

    A mechanically stable porous polymer membrane of Poly(vinylidene fluoride-hexafluoropropylene) has been prepared by phase inversion technique using steam as a non-solvent. The membrane possesses semicrystalline network with enhanced amorphicity as observed by X-ray diffraction. The membrane has been soaked in an electrolyte solution of 0.5M NaPF6 in Ethylene Carbonate/Propylene Carbonate (1:1) to obtain the gel polymer electrolyte. The porosity and electrolyte uptake of the membrane have been found to be 67% and 220% respectively. The room temperature ionic conductivity of the membrane has been obtained as ˜ 0.3 mS cm-1. The conductivity follows Arrhenius behavior with temperature and gives activation energy as 0.8 eV. The membrane has been found to possess significantly large electrochemical stability window of 5.0 V.

  5. Preparation of freestanding GaN wafer by hydride vapor phase epitaxy on porous silicon

    Science.gov (United States)

    Wu, Xian; Li, Peng; Liang, Renrong; Xiao, Lei; Xu, Jun; Wang, Jing

    2018-05-01

    A freestanding GaN wafer was prepared on porous Si (111) substrate using hydride vapor phase epitaxy (HVPE). To avoid undesirable effects of the porous surface on the crystallinity of the GaN, a GaN seed layer was first grown on the Si (111) bare wafer. A pattern with many apertures was fabricated in the GaN seed layer using lithography and etching processes. A porous layer was formed in the Si substrate immediately adjacent to the GaN seed layer by an anodic etching process. A 500-μm-thick GaN film was then grown on the patterned GaN seed layer using HVPE. The GaN film was separated from the Si substrate through the formation of cracks in the porous layer caused by thermal mismatch stress during the cooling stage of the HVPE. Finally, the GaN film was polished to obtain a freestanding GaN wafer.

  6. Preparation and hygrothermal properties of composite phase change humidity control materials

    International Nuclear Information System (INIS)

    Chen, Zhi; Qin, Menghao

    2016-01-01

    Highlights: • A new kind of phase change humidity control material (PCHCM) was prepared. • The PCHCM can moderate both the indoor temperature and humidity. • The silicon dioxide shell can improve the thermal properties of the composite. • The PCM microcapsules can improve the moisture buffer ability of the composite. • The CPCM/vesuvianite composite has a better hygrothermal performance than pure hygroscopic material. - Abstract: A novel phase change humidity control material (PCHCM) was prepared by using PCM microcapsules and different hygroscopic porous materials. The PCHCM composite can regulate the indoor hygrothermal environment by absorbing or releasing both heat and moisture. The PCM microcapsules were synthesized with methyl triethoxysilane by the sol–gel method. The vesuvianite, sepiolite and zeolite were used as hygroscopic materials. The scanning electron microscopy (SEM) was used to measure the morphology profiles of the microcapsules and PCHCM. The differential scanning calorimetry (DSC) and the thermal gravimetric analysis (TGA) were used to determine the thermal properties and thermal stability. Both the moisture transfer coefficient and moisture buffer value (MBV) of different PCHCMs were measured by the improved cup method. The DSC results showed that the SiO 2 shell can reduce the super-cooling degree of PCM. The super-cooling degrees of microcapsules and PCHCM are lower than that of the pure PCM. The onset temperature of thermal degradation of the microcapsules and PCHCMs is higher than that of pure PCM. Both the moisture transfer coefficient and MBV of PCHCMs are higher than that of the pure hygroscopic materials. The results indicated the PCHCMs have better thermal properties and moisture buffer ability.

  7. Preparation and Evaluation of Tretinoin Microemulsion Based on Pseudo-Ternary Phase Diagram

    Directory of Open Access Journals (Sweden)

    Fatemeh Leis

    2012-06-01

    Full Text Available Purpose: The aim of the present research was to formulate a transparent microemolsion as a topical delivery system for tretinoin for the treatment of acne. Methods: Microemulsion formulations prepared by mixing appropriate amount of surfactant including Tween 80 and Labrasol, co-surfactant such as propylene glycol (PG and oil phase including isopropyl myristate – transcutol P (10:1 ratio. The prepared microemolsions were evaluated regarding their particle size, zeta potential, conductivity, stability, viscosity, differential scanning calorimetry (DSC, scanning electron microscopy (SEM, refractory index (RI and pH. Results: The results showed that maximum oil was incorporated in microemolsion system that was contained surfactant to co-surfactant ratio (Km of 4:1. The mean droplets size range of microemulsion formulation were in the range of 14.1 to 36.5 nm and its refractory index (RI and pH were 1.46 and 6.1, respectively. Viscosity range was 200-350 cps. Drug release profile showed 49% of the drug released in the first 8 hours of experiment belong to ME-7. Also, Hexagonal and cubic structures were seen in the SEM photograph of the microemulsions. Conclusion: physicochemical properties and in vitro release were dependent upon the contents of S/C, water and, oil percentage in formulations.Also, ME-7 may be preferable for topical tretinoin formulation.

  8. Preparation of ultrafiltration membrane by phase separation coupled with microwave irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Suryani, Puput Eka [Department of Chemical Engineering, Faculty of Engineering, Diponegoro University Jl. Prof. Soedarto, Semarang 50275, Central Java (Indonesia); Department of Chemical Engineering, Faculty of Engineering, UniversitasMuhammadiyah Surakarta Jl. Jendral Ahmad Yani, Surakarta 57102, Central Java (Indonesia); Purnama, Herry [Department of Chemical Engineering, Faculty of Engineering, UniversitasMuhammadiyah Surakarta Jl. Jendral Ahmad Yani, Surakarta 57102, Central Java (Indonesia); Susanto, Heru, E-mail: heru.susanto@undip.ac.id [Department of Chemical Engineering, Faculty of Engineering, Diponegoro University Jl. Prof. Soedarto, Semarang 50275, Central Java (Indonesia)

    2015-12-29

    Preparation of low fouling ultrafiltration membrane is still a big challenge in the membrane field. In this paper, polyether sulfone (PES) ultrafiltration membranes were prepared by non-solvent-induced phase separation (NIPS) coupled with microwave irradiation. Polyethylene glycol (PEG) and polyethylene glycol methacrylate (PEGMA) were used as additives to improve membrane hydrophilicity. In this study, the concentration of additive, irradiation time and microwave power was varied. The membranes were characterized by scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy, while the performances were tested by adsorptive and ultrafiltration fouling experiments. The results show that the irradiation time and irradiation power are very important parameter that influence the membrane characteristic. In addition, type and concentration of additive are other important parameters. The results suggest that microwave irradiation is the most important parameter influencing the membrane characteristic. Both pure water flux and fouling resistance increase with increasing irradiation time, power irradiation, and additive concentration. PES membrane with addition of 10% w/w PEG and irradiated by 130 W microwave power for 180 seconds is the best membrane performance.

  9. Solid phase extraction for sample preparation in trace analysis of ionogenic compounds by capillary isotachophoresis

    International Nuclear Information System (INIS)

    Hutta, M.; Kaniansky, D.; Simunicova, E.; Zelenska, V.; Madajova, V.; Siskova, A.

    1992-01-01

    Various sorbents recommended for solid phase extraction (SPE) in sample preparation procedures were studied for use in combination with capillary isotachophoresis (ITP). They were very efficient in achieving trace concentration levels (low ppb, i.e., low parts per 10 9 ) for different types of ITP analytes present in environmental and biological matrices. A macroporous carbon sorbent was convenient for sample preparation in ITP analysis of short chain fatty acids (C 4 -C 9 ) in drinking water. Chelating sorbents based on hydroxyalkyl methacrylate matrix with salicylate, thioglycolate and 8-hydroxyquinolinate functionalities were found to be very suitable for preconcentration of heavy metals with an inherent sample clean-up. An octadecyl-bonded silica sorbent enabled in ITP a photometric detection of γ-aminobutyrate (labeled with a 2,4,6-trinitrophenyl group) at concentrations considerably lower than required for the determination of this amino acid in cerebrospinal fluid (∼5*10 -8 mol/l). (author) 34 refs.; 3 figs.; 1 tab

  10. An Approach to Preparing Ni-P with Different Phases for Use as Supercapacitor Electrode Materials.

    Science.gov (United States)

    Wang, Dan; Kong, Ling-Bin; Liu, Mao-Cheng; Luo, Yong-Chun; Kang, Long

    2015-12-01

    Herein, we describe a simple two-step approach to prepare nickel phosphide with different phases, such as Ni2 P and Ni5 P4 , to explain the influence of material microstructure and electrical conductivity on electrochemical performance. In this approach, we first prepared a Ni-P precursor through a ball milling process, then controlled the synthesis of either Ni2 P or Ni5 P4 by the annealing method. The as-prepared Ni2 P and Ni5 P4 are investigated as supercapacitor electrode materials for potential energy storage applications. The Ni2 P exhibits a high specific capacitance of 843.25 F g(-1) , whereas the specific capacitance of Ni5 P4 is 801.5 F g(-1) . Ni2 P possesses better cycle stability and rate capability than Ni5 P4 . In addition, the Fe2 O3 //Ni2 P supercapacitor displays a high energy density of 35.5 Wh kg(-1) at a power density of 400 W kg(-1) and long cycle stability with a specific capacitance retention rate of 96 % after 1000 cycles, whereas the Fe2 O3 //Ni5 P4 supercapacitor exhibits a high energy density of 29.8 Wh kg(-1) at a power density of 400 W kg(-1) and a specific capacitance retention rate of 86 % after 1000 cycles. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. On-line comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for preparative isolation of Peucedanum praeruptorum.

    Science.gov (United States)

    Wang, Xin-Yuan; Li, Jia-Fu; Jian, Ya-Mei; Wu, Zhen; Fang, Mei-Juan; Qiu, Ying-Kun

    2015-03-27

    A new on-line comprehensive preparative two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was developed for the separation of complicated natural products. It was based on the use of a silica gel packed medium-pressure column as the first dimension and an ODS preparative HPLC column as the second dimension. The two dimensions were connected with normal-phase (NP) and reversed-phase (RP) enrichment units, involving a newly developed airflow assisted adsorption (AAA) technique. The instrument operation and the performance of this NPLC × RPLC separation method were illustrated by gram-scale isolation of ethanol extract from the roots of Peucedanum praeruptorum. In total, 19 compounds with high purity were obtained via automated multi-step preparative separation in a short period of time using this system, and their structures were comprehensively characterized by ESI-MS, (1)H NMR, and (13)C NMR. Including two new compounds, five isomers in two groups with identical HPLC and TLC retention values were also obtained and identified by 1D NMR and 2D NMR. This is the first report of an NPLC × RPLC system successfully applied in an on-line preparative process. This system not only solved the interfacing problem of mobile-phase immiscibility caused by NP and RP separation, it also exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Preparation of graphene/TiO2 composites by nonionic surfactant strategy and their simulated sunlight and visible light photocatalytic activity towards representative aqueous POPs degradation

    International Nuclear Information System (INIS)

    Li, Kexin; Xiong, Jingjing; Chen, Tong; Yan, Liushui; Dai, Yuhua; Song, Dongyang; Lv, Ying; Zeng, Zhenxing

    2013-01-01

    Highlights: ► A series of graphene/TiO 2 composites were developed by nonionic surfactant strategy. ► The textural property, optical property, and composition were well characterized. ► Aqueous POPs were degraded under simulated sunlight and visible light irradiation. ► The degradation mechanism and kinetics of aqueous POPs were studied in detail. ► Mineralization of aqueous POPs and recyclability of the composites were also tested. -- Abstract: A series of graphene/TiO 2 composites were fabricated using a single-step nonionic surfactant strategy combined with the solvothermal treatment technique. Their phase structure, morphology, porosity, optical absorption property, as well as composition and structure, were characterized. The as-prepared composites were successfully applied to degrade aqueous persistent organic pollutants (POPs) such as rhodamine B, aldicarb, and norfloxacin in simulated sunlight (λ > 320 nm) and visible light (λ > 400 nm) irradiation. The degradation mechanism and kinetics of aqueous POPs were studied in detail. The mineralization of aqueous POPs and the recyclability of the composites were also tested in the same condition

  13. Dynamics of cation ordering in an intentionally prepared low-Tc pseudocubic NdBa2Cu3O6.9 phase

    International Nuclear Information System (INIS)

    Goodilin, E A; Peryshkov, D V; Didenko, K V; Makarova, M V; Tretyakov, Yu D

    2004-01-01

    The modification of a NdBa 2 Cu 3 O 6.9 superconductor representing its disordered state with a low T c ∼ 50K and a pseudocubic a∼ b ∼ c/3 ∼3.9 A unit cell was prepared reproducibly from freeze-dried nitrate precursors. Isothermal annealing of the pseudocubic phase for 60-70 h at ∼1000 C in air converted it gradually into the conventional modification with a T c ∼ 90K and a regular orthorhombic lattice after oxygenation

  14. The preparation of Zr-deuteride and phase stability studies of the Zr-D system

    Science.gov (United States)

    Maimaitiyili, T.; Steuwer, A.; Bjerkén, C.; Blomqvist, J.; Hoelzel, M.; Ion, J. C.; Zanellato, O.

    2017-03-01

    Deuteride phases in the zirconium-deuterium system in the temperature range 25-286 °C have been studied in-situ by high resolution neutron diffraction. The study primarily focused on observations of δ→γ transformation at 180 °C, and the peritectoid reaction α + δ ↔ γ at 255 °C in commercial grade Zr powder that was deuterated to a deuterium/Zr ratio of one to one. A detailed description of the zirconium deuteride preparation route by high temperature gas loading is also described. The lattice parameters of α-Zr, δ-ZrDx and ε-ZrDx were determined by whole pattern crystal structure analysis, using Rietveld and Pawley refinements, and are in good agreement with values reported in the literature. The controversial γ-hydride phase was observed both in-situ and ex-situ in deuterated Zr powder after a heat treatment at 286 °C and slow cooling.

  15. Preparation of nanoencapsulated phase change material as latent functionally thermal fluid

    Energy Technology Data Exchange (ETDEWEB)

    Fang Yutang; Kuang Shengyan; Gao Xuenong; Zhang Zhengguo, E-mail: ppytfang@scut.edu.c [Key Laboratory of Enhanced Heat Transfer and Energy Conservation, Ministry of Education, South China University of Technology, Guangzhou 510640 (China)

    2009-02-07

    Nanoencapsulated phase change material with polystyrene as the shell and n-octadecane as the core was synthesized using the ultrasonic technique and miniemulsion in situ polymerization. The influences of polymerization factors, including initiator, chain transfer agent (CTA), surfactant, n-octadecane/styrene ratio and hydrophilic co-monomer, on the morphology and thermophysical properties of nanocapsules were systematically investigated. The optimized polymerization conditions were 0.5 wt% of initiator (2,2-azobisisobutyronitrile), 0.4 wt% of CTA (n-dodecyl mercaptan), 2% of composite surfactants which were composed of sodium dodecyl sulfate and poly-(ethylene glycol) monooctylphenyl ether by 1 : 1 in weight ratio, 1 wt% of hydrophilic co-monomer butyl acrylate or 3 wt% of methyl methacrylate and 1 : 1 n-octadecane to styrene in weight ratio. Under these conditions, the z-average size of prepared nanocapsules was 124 nm and the phase change enthalpy was 124.4 kJ kg{sup -1}. The heat capacity was as high as 11.61 kJ kg{sup -1} K{sup -1} at the latex concentration of 20.6 wt%. Thermal stability and viscosity testing show that this fluid had excellent resistance to thermal shock (after 100 cycles, no liquid Oct was observed during heating) and low viscosity (only 3.61 mPa s at the latex concentration of 20.6 wt%), which seems to be promising as a latent functionally thermal fluid.

  16. Preparation, characterization, and thermal properties of microencapsulated phase change material for thermal energy storage

    Energy Technology Data Exchange (ETDEWEB)

    Alkan, Cemil; Sari, Ahmet; Karaipekli, Ali [Department of Chemistry, Gaziosmanpasa University, 60240 Tokat (Turkey); Uzun, Orhan [Department of Physics, Gaziosmanpasa University, 60240 Tokat (Turkey)

    2009-01-15

    This study is focused on the preparation, characterization, and determination of thermal properties of microencapsulated docosane with polymethylmethacrylate (PMMA) as phase change material for thermal energy storage. Microencapsulation of docosane has been carried out by emulsion polymerization. The microencapsulated phase change material (MEPCM) was characterized using scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR) spectroscopy. Thermal properties and thermal stability of MEPCM were measured by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). DSC analysis indicated that the docosane in the microcapsules melts at 41.0 C and crystallizes at 40.6 C. It has latent heats of 54.6 and -48.7 J/g for melting and crystallization, respectively. TGA showed that the MEPCM degraded in three distinguishable steps and had good chemical stability. Accelerated thermal cycling tests also indicated that the MEPCM had good thermal reliability. Based on all these results, it can be concluded that the microencapsulated docosane as MEPCMs have good potential for thermal energy storage purposes such as solar space heating applications. (author)

  17. [Nasal submicron emulsion of Scutellariae Radix extract preparation technology research based on phase transfer of solute technology].

    Science.gov (United States)

    Shi, Ya-jun; Shi, Jun-hui; Chen, Shi-bin; Yang, Ming

    2015-07-01

    Based on the demand of nasal drug delivery high drug loadings, using the unique phase transfer of solute, integrating the phospholipid complex preparation and submicron emulsion molding process of Scutellariae Radix extract, the study obtained the preparation of the high drug loadings submicron emulsion of Scutellariae Radix extract. In the study of drug solution dispersion method, the uniformity of drug dispersed as the evaluation index, the traditional mixing method, grinding, homogenate and solute phase transfer technology were investigated, and the solute phase transfer technology was adopted in the last. With the adoption of new technology, the drug loading capacity reached 1.33% (phospholipid complex was 4%). The drug loading capacity was improved significantly. The transfer of solute method and timing were studied as follows,join the oil phase when the volume of phospholipid complex anhydrous ethanol solution remaining 30%, the solute phase transfer was completed with the continued recycling of anhydrous ethanol. After drug dissolved away to oil phase, the preparation technology of colostrum was determined with the evaluation index of emulsion droplet form. The particle size of submicron emulsion, PDI and stability parameters were used as evaluation index, orthogonal methodology were adopted to optimize the submicron emulsion ingredient and main influential factors of high pressure homogenization technology. The optimized preparation technology of Scutellariae Radix extract nasal submicron emulsion is practical and stable.

  18. Phase composition and tribomechanical properties of Ti-B-C nanocomposite coatings prepared by magnetron sputtering

    International Nuclear Information System (INIS)

    Sánchez-López, J C; Abad, M D; Justo, A; Gago, R; Endrino, J L; García-Luis, A; Brizuela, M

    2012-01-01

    Protective nanocomposite coatings based on hard ceramic phases (TiC, TiB 2 ) combined with amorphous carbon (a-C) are of interest because of their adequate balance between mechanical and tribological performances. In this work, Ti-B-C nanocomposite coatings were prepared by co-sputtering of graphite and TiB 2 targets. Varying the discharge power ratio applied to the graphite and TiB 2 targets from 0 to 2, the a-C content in the coatings could be tuned from 0 to 60%, as observed by means of Raman and x-ray photoelectron spectroscopy (XPS). The microstructural characterization demonstrated a progressive decrease in crystallinity from an initial nanocrystalline (nc) TiB 2 -like structure to a distorted TiB x C y ternary compound with increasing C concentration. X-ray absorption near-edge structure measurements on the B K-edge helped to determine a hexagonal arrangement around the B atoms in the ternary TiB x C y phase. A fitting analysis of the C 1s XPS peak allowed us to evaluate the relative amount of a-C and TiB x C y components. A drastic change in hardness (from 52 to 13 GPa) and friction coefficient values (from 0.8 to 0.2) is noticed when moving from nc-TiB 2 to TiBC/a-C nanocomposites. The fraction of a-C necessary to decrease the friction below 0.2 was found to be 45%. Raman observation of the wear tracks determined the presence of disordered sp 2 -bonded carbon phase associated with the diminution of the friction level.

  19. The preparation of Zr-deuteride and phase stability studies of the Zr-D system

    Energy Technology Data Exchange (ETDEWEB)

    Maimaitiyili, T., E-mail: tuerdi.maimaitiyili@mah.se [Materials Science and Applied Mathematics, Malmö University, Nordenskiöldsgatan 1, 20506 Malmö (Sweden); Steuwer, A. [Nelson Mandela Metropolitan University, Gardham Avenue, 6031 Port Elizabeth (South Africa); Bjerkén, C.; Blomqvist, J. [Materials Science and Applied Mathematics, Malmö University, Nordenskiöldsgatan 1, 20506 Malmö (Sweden); Hoelzel, M. [Forschungsneutronenquelle Heinz-Maier-Leibnitz (FRM II), Technische Universität Muünchen, Lichtenbergstr. 1, D-85747 Garching (Germany); Ion, J.C. [Materials Science and Applied Mathematics, Malmö University, Nordenskiöldsgatan 1, 20506 Malmö (Sweden); Zanellato, O. [PIMM, Ensam - Cnam - CNRS, 151 Boulevard de l' Hôpital, 75013 Paris (France)

    2017-03-15

    Deuteride phases in the zirconium-deuterium system in the temperature range 25–286 °C have been studied in-situ by high resolution neutron diffraction. The study primarily focused on observations of δ→γ transformation at 180 °C, and the peritectoid reaction α + δ ↔ γ at 255 °C in commercial grade Zr powder that was deuterated to a deuterium/Zr ratio of one to one. A detailed description of the zirconium deuteride preparation route by high temperature gas loading is also described. The lattice parameters of α-Zr, δ-ZrD{sub x} and ε-ZrD{sub x} were determined by whole pattern crystal structure analysis, using Rietveld and Pawley refinements, and are in good agreement with values reported in the literature. The controversial γ-hydride phase was observed both in-situ and ex-situ in deuterated Zr powder after a heat treatment at 286 °C and slow cooling. - Highlights: • Controversial γ phase observed both in-situ and ex-situ after heat treatments. • γ-ZrD is observed at room temperature after 5 h of heat treatment at 286 °C. • Presence of α + δ ↔ γ at 255 °C was not observed. • It was observed that there is a δ → γ transformation present around 150 °C.

  20. Phase composition and tribomechanical properties of Ti-B-C nanocomposite coatings prepared by magnetron sputtering

    Science.gov (United States)

    Sánchez-López, J. C.; Abad, M. D.; Justo, A.; Gago, R.; Endrino, J. L.; García-Luis, A.; Brizuela, M.

    2012-09-01

    Protective nanocomposite coatings based on hard ceramic phases (TiC, TiB2) combined with amorphous carbon (a-C) are of interest because of their adequate balance between mechanical and tribological performances. In this work, Ti-B-C nanocomposite coatings were prepared by co-sputtering of graphite and TiB2 targets. Varying the discharge power ratio applied to the graphite and TiB2 targets from 0 to 2, the a-C content in the coatings could be tuned from 0 to 60%, as observed by means of Raman and x-ray photoelectron spectroscopy (XPS). The microstructural characterization demonstrated a progressive decrease in crystallinity from an initial nanocrystalline (nc) TiB2-like structure to a distorted TiBxCy ternary compound with increasing C concentration. X-ray absorption near-edge structure measurements on the B K-edge helped to determine a hexagonal arrangement around the B atoms in the ternary TiBxCy phase. A fitting analysis of the C 1s XPS peak allowed us to evaluate the relative amount of a-C and TiBxCy components. A drastic change in hardness (from 52 to 13 GPa) and friction coefficient values (from 0.8 to 0.2) is noticed when moving from nc-TiB2 to TiBC/a-C nanocomposites. The fraction of a-C necessary to decrease the friction below 0.2 was found to be 45%. Raman observation of the wear tracks determined the presence of disordered sp2-bonded carbon phase associated with the diminution of the friction level.

  1. Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Luo Fan [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China); Wu Zucheng [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China)], E-mail: wuzc@zju.edu.cn; Tao Ping [Institute of Structural Mechanics, China Academy of Engineering Physics, Mianyang 621900 (China); Cong Yanqing [College of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China)

    2009-01-05

    Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 {mu}g L{sup -1}, the linear ranges were between 0.6 and 35619 {mu}g L{sup -1} with good linearity (R{sup 2} = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

  2. Advanced fabrication method for the preparation of MOF thin films: Liquid-phase epitaxy approach meets spin coating method.

    KAUST Repository

    Chernikova, Valeriya

    2016-07-14

    Here we report a new and advanced method for the fabrication of highly oriented/polycrystalline metal-organic framework (MOF) thin films. Building on the attractive features of the liquid-phase epitaxy (LPE) approach, a facile spin coating method was implemented to generate MOF thin films in a high-throughput fashion. Advantageously, this approach offers a great prospective to cost-effectively construct thin-films with a significantly shortened preparation time and a lessened chemicals and solvents consumption, as compared to the conventional LPE-process. Certainly, this new spin-coating approach has been implemented successfully to construct various MOF thin films, ranging in thickness from a few micrometers down to the nanometer scale, spanning 2-D and 3-D benchmark MOF materials including Cu2(bdc)2•xH2O, Zn2(bdc)2•xH2O, HKUST-1 and ZIF-8. This method was appraised and proved effective on a variety of substrates comprising functionalized gold, silicon, glass, porous stainless steel and aluminum oxide. The facile, high-throughput and cost-effective nature of this approach, coupled with the successful thin film growth and substrate versatility, represents the next generation of methods for MOF thin film fabrication. Thereby paving the way for these unique MOF materials to address a wide range of challenges in the areas of sensing devices and membrane technology.

  3. Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

    International Nuclear Information System (INIS)

    Catalá-Icardo, M.; Torres-Cartas, S.; Meseguer-Lloret, S.; Gómez-Benito, C.; Carrasco-Correa, E.; Simó-Alfonso, E.F.; Ramis-Ramos, G.; Herrero-Martínez, J.M.

    2017-01-01

    In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch"®), or mixtures of H_2O_2 and H_2SO_4, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the tubing wall and the stable anchorage of monolith to the wall, respectively. Special emphasis was also put on the reduction of the unwanted effects of shrinking of monolith during polymerization, by using an external proper mold and by selecting the adequate monomers in order to increase the flexibility of the polymer. Poly(glycidyl methacrylate-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface-vinylized PTFE tubes. The modified PTFE tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 20 MPa. The column performance was also evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode. The optimized monolithic columns gave plate heights ranged between 70 and 80 μm. The resulting monoliths were also satisfactorily applied to the separation of proteins. - Highlights: • Successful surface etching of PTFE inner wall tubing was done. • The modified PTFE support was next methacryloylated with GMA. • Organic polymeric monolith was in situ prepared in the functionalized PTFE tube. • The monolithic columns gave suitable pressure resistance and separation of proteins.

  4. Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Catalá-Icardo, M., E-mail: mocaic@qim.upv.es [Research Institute for Integrated Management of Coastal Areas, Universitat Politècnica de València, Paranimf 1, 46730, Grao de Gandía, Valencia (Spain); Torres-Cartas, S.; Meseguer-Lloret, S.; Gómez-Benito, C. [Research Institute for Integrated Management of Coastal Areas, Universitat Politècnica de València, Paranimf 1, 46730, Grao de Gandía, Valencia (Spain); Carrasco-Correa, E.; Simó-Alfonso, E.F.; Ramis-Ramos, G. [Department of Analytical Chemistry, Universitat de València, Dr. Moliner 50, 46100, Burjassot, Valencia (Spain); Herrero-Martínez, J.M., E-mail: jmherrer@uv.es [Department of Analytical Chemistry, Universitat de València, Dr. Moliner 50, 46100, Burjassot, Valencia (Spain)

    2017-04-01

    In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch{sup ®}), or mixtures of H{sub 2}O{sub 2} and H{sub 2}SO{sub 4}, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the tubing wall and the stable anchorage of monolith to the wall, respectively. Special emphasis was also put on the reduction of the unwanted effects of shrinking of monolith during polymerization, by using an external proper mold and by selecting the adequate monomers in order to increase the flexibility of the polymer. Poly(glycidyl methacrylate-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface-vinylized PTFE tubes. The modified PTFE tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 20 MPa. The column performance was also evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode. The optimized monolithic columns gave plate heights ranged between 70 and 80 μm. The resulting monoliths were also satisfactorily applied to the separation of proteins. - Highlights: • Successful surface etching of PTFE inner wall tubing was done. • The modified PTFE support was next methacryloylated with GMA. • Organic polymeric monolith was in situ prepared in the functionalized PTFE tube. • The monolithic columns gave suitable pressure resistance and separation of proteins.

  5. Electrical, optical, and structural properties of GaN films prepared by hydride vapor phase epitaxy

    International Nuclear Information System (INIS)

    Polyakov, A.Y.; Smirnov, N.B.; Yakimov, E.B.; Usikov, A.S.; Helava, H.; Shcherbachev, K.D.; Govorkov, A.V.; Makarov, Yu N.; Lee, In-Hwan

    2014-01-01

    Highlights: • GaN films are prepared by hydride vapor phase epitaxy (HVPE). • Residual donors and deep traps show a minimum density versus growth temperature. • This minimum is located close to the HVPE growth temperature of 950 °C. • Good crystalline GaN with residual donor density < 10 16 cm −3 can be grown at 950 °C. - Abstract: Two sets of undoped GaN films with the thickness of 10–20 μm were prepared by hydride vapor phase epitaxy (HVPE) and characterized by capacitance–voltage (C–V) profiling, microcathodoluminescence (MCL) spectra measurements, MCL imaging, electron beam induced current (EBIC) imaging, EBIC dependence on accelerating voltage, deep levels transient spectroscopy, high resolution X-ray diffraction measurements. The difference in growth conditions was mainly related to the lower (850 °C, group 1) or higher (950 °C, group 2) growth temperature. Both groups of samples showed similar crystalline quality with the dislocation density close to 10 8 cm −2 , but very different electrical and optical properties. In group 1 samples the residual donors concentration was ∼10 17 cm −3 or higher, the MCL spectra were dominated by the band-edge luminescence, and the diffusion length of charge carriers was close to 0.1 μm. Group 2 samples had a 2–4.5 μm thick highly resistive layer on top, for which MCL spectra were determined by green, yellow and red defect bands, and the diffusion length was 1.5 times higher than in group 1. We also present brief results of growth at the “standard” HVPE growth temperature of 1050 °C that show the presence of a minimum in the net donor concentration and deep traps density as a function of the growth temperature. Possible reasons for the observed results are discussed in terms of the electrical compensation of residual donors by deep traps

  6. Preparation and characterization of a new microwave immobilized poly(2-phenylpropyl)methylsiloxane stationary phase for reversed phase high-performance liquid chromatography.

    Science.gov (United States)

    Begnini, Fernanda R; Jardim, Isabel C S F

    2013-07-05

    A new reversed phase high-performance liquid chromatography (RP-HPLC) stationary phase was prepared and its chromatographic and physical-chemical properties were evaluated. The new stationary phase was prepared with a silica support and poly(2-phenylpropyl)methylsiloxane (PPPMS), a phenyl type polysiloxane copolymer. Since this is a new copolymer and there is little information in the literature, it was submitted to physical-chemical characterization by infrared spectroscopy and thermogravimetry. The chromatographic phase was prepared through sorption and microwave immobilization of the copolymer onto a silica support. The chromatographic performance was evaluated by employing test procedures suggested by Engelhardt and Jungheim, Tanaka and co-workers, Neue, and Szabó and Csató. These test mixtures provide information about the hydrophobic selectivity, silanophilic activity, ion-exchange capacity, shape selectivity and interaction with polar analytes of the new Si-PPPMS reversed phase. Stability tests were developed using accelerated aging tests under both basic and acidic conditions to provide information about the lifetime of the packed columns. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. EX8000 ramps up preparation phase in Horizon oil sands project

    Energy Technology Data Exchange (ETDEWEB)

    Anon.

    2006-07-15

    This article presented details of Hitachi's EX8000 hydraulic shovel, a key piece of equipment that will be used throughout the extensive mine preparation phase of the Horizon oil sands project. Within 2 years, the project expects to produce over 200,000 barrels of oil per day. However, more than 400 million cubic metres of soil will need to be moved before production can begin. In order to remain on schedule, overburden must be removed in massive volumes. With a 52.3 cubic yard bucket, the Hitachi EX8000 has the capacity to feed a dozen 320 metric tonne haul trucks as well as several smaller 282 metric tonne trucks, and can fill each truck in 4 passes. Material is now being moved by to an area in which dikes are being constructed to house water generated in the refining process. Stockpiling, relocation and reclamation phases will follow as the project progresses. In order to reach the oil, as much as 75 feet of overburden must be removed, including layers of sandstone, limestone, trap rock and other materials. Once the overburden has been removed, oil sand layers are also often intermixed with other materials. The EX8000 can separate the tramp material from the oil sands, improving the overall efficiency of the operation. The Alberta-based North American Construction Group, who have a 10-year contract with Canadian Natural Resources Ltd. for the Horizon project, owns more than 100 Hitachi units in various sizes and has already purchased another EX8000 which is slated for delivery in the Fall of 2006. It was concluded that the company has purchased hundreds of new trucks to handle added volumes of materials being moved as the oil sands industry gains momentum. 3 figs.

  8. RPA accumulation during class switch recombination represents 5'-3' DNA-end resection during the S-G2/M phase of the cell cycle.

    Science.gov (United States)

    Yamane, Arito; Robbiani, Davide F; Resch, Wolfgang; Bothmer, Anne; Nakahashi, Hirotaka; Oliveira, Thiago; Rommel, Philipp C; Brown, Eric J; Nussenzweig, Andre; Nussenzweig, Michel C; Casellas, Rafael

    2013-01-31

    Activation-induced cytidine deaminase (AID) promotes chromosomal translocations by inducing DNA double-strand breaks (DSBs) at immunoglobulin (Ig) genes and oncogenes in the G1 phase. RPA is a single-stranded DNA (ssDNA)-binding protein that associates with resected DSBs in the S phase and facilitates the assembly of factors involved in homologous repair (HR), such as Rad51. Notably, RPA deposition also marks sites of AID-mediated damage, but its role in Ig gene recombination remains unclear. Here, we demonstrate that RPA associates asymmetrically with resected ssDNA in response to lesions created by AID, recombination-activating genes (RAG), or other nucleases. Small amounts of RPA are deposited at AID targets in G1 in an ATM-dependent manner. In contrast, recruitment in the S-G2/M phase is extensive, ATM independent, and associated with Rad51 accumulation. In the S-G2/M phase, RPA increases in nonhomologous-end-joining-deficient lymphocytes, where there is more extensive DNA-end resection. Thus, most RPA recruitment during class switch recombination represents salvage of unrepaired breaks by homology-based pathways during the S-G2/M phase of the cell cycle. Copyright © 2013 The Authors. Published by Elsevier Inc. All rights reserved.

  9. Preparation and thermal energy storage properties of paraffin/calcined diatomite composites as form-stable phase change materials

    International Nuclear Information System (INIS)

    Sun, Zhiming; Zhang, Yuzhong; Zheng, Shuilin; Park, Yuri; Frost, Ray L.

    2013-01-01

    Highlights: ► Composite phase change material (PCM) was prepared by blending composite paraffin and calcined diatomite. ► The optimum mixed proportion was obtained through differential scanning calorimetry. ► Thermal energy storage properties of the composite PCMs were determined by DSC. ► Thermal cycling test showed that the prepared PCMs are thermally reliable and chemically stable. - Abstract: A composite paraffin-based phase change material (PCM) was prepared by blending composite paraffin and calcined diatomite through the fusion adsorption method. In this study, raw diatomite was purified by thermal treatment in order to improve the adsorption capacity of diatomite, which acted as a carrier material to prepare shape-stabilized PCMs. Two forms of paraffin (paraffin waxes and liquid paraffin) with different melting points were blended together by the fusion method, and the optimum mixed proportion with a suitable phase-transition temperature was obtained through differential scanning calorimetry (DSC) analysis. Then the prepared composite paraffin was adsorbed in calcined diatomite. The prepared paraffin/calcined diatomite composites were characterized by the scanning electron microscope (SEM) and Fourier transformation infrared (FT-IR) analysis techniques. Thermal energy storage properties of the composite PCMs were determined by DSC method. DSC results showed that there was an optimum adsorption ratio between composite paraffin and calcined diatomite and the phase-transition temperature and the latent heat of the composite PCMs were 33.04 °C and 89.54 J/g, respectively. Thermal cycling test of composite PCMs showed that the prepared material is thermally reliable and chemically stable. The obtained paraffin/calcined diatomite composites have proper latent heat and melting temperatures, and show practical significance and good potential application value

  10. Preparation and thermal energy storage properties of paraffin/calcined diatomite composites as form-stable phase change materials

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Zhiming [School of Chemical and Environmental Engineering, China University of Mining and Technology, Beijing 100083 (China); Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Zhang, Yuzhong [School of Chemical and Environmental Engineering, China University of Mining and Technology, Beijing 100083 (China); Zheng, Shuilin, E-mail: shuilinzh@yahoo.com.cn [School of Chemical and Environmental Engineering, China University of Mining and Technology, Beijing 100083 (China); Park, Yuri [Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Frost, Ray L., E-mail: r.frost@qut.edu.au [Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane, Queensland 4001 (Australia)

    2013-04-20

    Highlights: ► Composite phase change material (PCM) was prepared by blending composite paraffin and calcined diatomite. ► The optimum mixed proportion was obtained through differential scanning calorimetry. ► Thermal energy storage properties of the composite PCMs were determined by DSC. ► Thermal cycling test showed that the prepared PCMs are thermally reliable and chemically stable. - Abstract: A composite paraffin-based phase change material (PCM) was prepared by blending composite paraffin and calcined diatomite through the fusion adsorption method. In this study, raw diatomite was purified by thermal treatment in order to improve the adsorption capacity of diatomite, which acted as a carrier material to prepare shape-stabilized PCMs. Two forms of paraffin (paraffin waxes and liquid paraffin) with different melting points were blended together by the fusion method, and the optimum mixed proportion with a suitable phase-transition temperature was obtained through differential scanning calorimetry (DSC) analysis. Then the prepared composite paraffin was adsorbed in calcined diatomite. The prepared paraffin/calcined diatomite composites were characterized by the scanning electron microscope (SEM) and Fourier transformation infrared (FT-IR) analysis techniques. Thermal energy storage properties of the composite PCMs were determined by DSC method. DSC results showed that there was an optimum adsorption ratio between composite paraffin and calcined diatomite and the phase-transition temperature and the latent heat of the composite PCMs were 33.04 °C and 89.54 J/g, respectively. Thermal cycling test of composite PCMs showed that the prepared material is thermally reliable and chemically stable. The obtained paraffin/calcined diatomite composites have proper latent heat and melting temperatures, and show practical significance and good potential application value.

  11. Preparation and Thermal Properties of Eutectic Hydrate Salt Phase Change Thermal Energy Storage Material

    Directory of Open Access Journals (Sweden)

    Lin Liang

    2018-01-01

    Full Text Available In this study, a new cold storage phase change material eutectic hydrate salt (K2HPO4·3H2O–NaH2PO4·2H2O–Na2S2O3·5H2O was prepared, modified, and tested. The modification was performed by adding a nucleating agent and thickener. The physical properties such as viscosity, surface tension, cold storage characteristics, supercooling, and the stability during freeze-thaw cycles were studied. Results show that the use of nucleating agents, such as sodium tetraborate, sodium fluoride, and nanoparticles, are effective. The solidification temperature and latent heat of these materials which was added with 0, 3, and 5 wt% thickeners were −11.9, −10.6, and −14.8°C and 127.2, 118.6, 82.56 J/g, respectively. Adding a nucleating agent can effectively improve the nucleation rate and nucleation stability. Furthermore, increasing viscosity has a positive impact on the solidification rate, supercooling, and the stability during freeze-thaw cycles.

  12. Preparation and flow characteristic of a novel phase change fluid for latent heat transfer

    Energy Technology Data Exchange (ETDEWEB)

    Zou, Deqiu [Marine College of Ningbo University, Ningbo 315211, Zhejiang (China); Guangzhou Institute of Energy Conversion, Chinese Academy of Sciences, Guangzhou 510640 (China); Feng, Ziping; Xiao, Rui; Qin, Kun; Zhang, Jianjun; Song, Wenji; Tu, Qiu [Guangzhou Institute of Energy Conversion, Chinese Academy of Sciences, Guangzhou 510640 (China)

    2010-12-15

    A novel phase change emulsion (PCE) was prepared and its latent heat was measured by DSC. To analyze its feasibility in heat transportation through a piping system, an experimental system was built. The pressure drop of the PCE for turbulent flow was measured and the effects of such facts as the paraffin concentration and flow velocity were discussed. According to the pressure characteristic and latent heat of the PCE, the pumping power consumption rates of PCE to water under the same pipe diameter and a given heat transportation quantity can be obtained. The results show that mass flow rate and pumping power consumption of the PCE decrease greatly compared with water. For example, the decrease can be up to about 73% at V=0.6 m/s (20 and 30 wt%). Furthermore, the results show that PCE of 20 wt% can obtain almost the same pumping power consumption savings as PCE of 30 wt% in a certain flow velocity range. Finally, the applications of the PCE in the area of waste heat usage, electrical boiler and solar energy usage were commented. (author)

  13. Impact of column and stationary phase properties on the productivity in chiral preparative LC.

    Science.gov (United States)

    Forssén, Patrik; Fornstedt, Torgny

    2018-03-01

    By generating 1500 random chiral separation systems, assuming two-site Langmuir interactions, we investigated numerically how the maximal productivity (P R,max ) was affected by changes in stationary phase adsorption properties. The relative change in P R,max , when one adsorption property changed 10%, was determined for each system and for each studied parameter the corresponding productivity change distribution of the systems was analyzed. We could conclude that there is no reason to have columns with more than 500 theoretical plates and larger selectivity than 3. More specifically, we found that changes in selectivity have a major impact on P R,max if it is below ∼2 and, interestingly, increasing selectivity when it is above ∼3 decreases P R,max . Increase in relative saturation capacity will have a major impact on P R,max if it is below ∼40%, but only modest above this percent. Increasing total monolayer saturation capacity, or decreasing the first eluting enantiomer's retention factor, will have a modest effect on P R,max and increased efficiency will have almost no effect at all on P R,max unless it is below ∼500 theoretical plates. Finally, we showed that chiral columns with superior analytic performance might have inferior preparative performance, or vice versa. It is, therefore, not possible to assess columns based on their analytical performance alone. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Design and Preparation of Carbon Based Composite Phase Change Material for Energy Piles

    Directory of Open Access Journals (Sweden)

    Haibin Yang

    2017-04-01

    Full Text Available Energy piles—A fairly new renewable energy concept—Use a ground heat exchanger (GHE in the foundation piles to supply heating and cooling loads to the supported building. Applying phase change materials (PCMs to piles can help in maintaining a stable temperature within the piles and can then influence the axial load acting on the piles. In this study, two kinds of carbon-based composite PCMs (expanded graphite-based PCM and graphite nanoplatelet-based PCM were prepared by vacuum impregnation for potential application in energy piles. Thereafter, a systematic study was performed and different characterization tests were carried out on two composite PCMs. The composite PCMs retained up to 93.1% of paraffin and were chemically compatible, thermally stable and reliable. The latent heat of the composite PCM was up to 152.8 J/g while the compressive strength of cement paste containing 10 wt % GNP-PCM was found to be 37 MPa. Hence, the developed composite PCM has potential for thermal energy storage applications.

  15. Design and Preparation of Carbon Based Composite Phase Change Material for Energy Piles.

    Science.gov (United States)

    Yang, Haibin; Memon, Shazim Ali; Bao, Xiaohua; Cui, Hongzhi; Li, Dongxu

    2017-04-07

    Energy piles-A fairly new renewable energy concept-Use a ground heat exchanger (GHE) in the foundation piles to supply heating and cooling loads to the supported building. Applying phase change materials (PCMs) to piles can help in maintaining a stable temperature within the piles and can then influence the axial load acting on the piles. In this study, two kinds of carbon-based composite PCMs (expanded graphite-based PCM and graphite nanoplatelet-based PCM) were prepared by vacuum impregnation for potential application in energy piles. Thereafter, a systematic study was performed and different characterization tests were carried out on two composite PCMs. The composite PCMs retained up to 93.1% of paraffin and were chemically compatible, thermally stable and reliable. The latent heat of the composite PCM was up to 152.8 J/g while the compressive strength of cement paste containing 10 wt % GNP-PCM was found to be 37 MPa. Hence, the developed composite PCM has potential for thermal energy storage applications.

  16. Preparation and Optical Properties of Spherical Inverse Opals by Liquid Phase Deposition Using Spherical Colloidal Crystals

    International Nuclear Information System (INIS)

    Aoi, Y; Tominaga, T

    2013-01-01

    Titanium dioxide (TiO 2 ) inverse opals in spherical shape were prepared by liquid phase deposition (LPD) using spherical colloidal crystals as templates. Spherical colloidal crystals were produced by ink-jet drying technique. Aqueous emulsion droplets that contain polystyrene latex particles were ejected into air and dried. Closely packed colloidal crystals with spherical shape were obtained. The obtained spherical colloidal crystals were used as templates for the LPD. The templates were dispersed in the deposition solution of the LPD, i.e. a mixed solution of ammonium hexafluorotitanate and boric acid and reacted for 4 h at 30 °C. After the LPD process, the interstitial spaces of the spherical colloidal crystals were completely filled with titanium oxide. Subsequent heat treatment resulted in removal of templates and spherical titanium dioxide inverse opals. The spherical shape of the template was retained. SEM observations indicated that the periodic ordered voids were surrounded by titanium dioxide. The optical reflectance spectra indicated that the optical properties of the spherical titanium dioxide inverse opals were due to Bragg diffractions from the ordered structure. Filling in the voids of the inverse opals with different solvents caused remarkable changes in the reflectance peak.

  17. Preparation and Characterization of Microencapsulated Phase Change Materials for Use in Building Applications.

    Science.gov (United States)

    Giro-Paloma, Jessica; Al-Shannaq, Refat; Fernández, Ana Inés; Farid, Mohammed M

    2015-12-26

    A method for preparing and characterizing microencapsulated phase change materials (MPCM) was developed. A comparison with a commercial MPCM is also presented. Both MPCM contained paraffin wax as PCM with acrylic shell. The melting temperature of the PCM was around 21 °C, suitable for building applications. The M-2 (our laboratory made sample) and Micronal ® DS 5008 X (BASF) samples were characterized using SEM, DSC, nano-indentation technique, and Gas Chromatography/Mass spectrometry (GC-MS). Both samples presented a 6 μm average size and a spherical shape. Thermal energy storage (TES) capacities were 111.73 J·g -1 and 99.3 J·g -1 for M-2 and Micronal ® DS 5008 X, respectively. Mechanical characterization of the samples was performed by nano-indentation technique in order to determine the elastic modulus ( E ), load at maximum displacement ( P m ), and displacement at maximum load ( h m ), concluding that M-2 presented slightly better mechanical properties. Finally, an important parameter for considering use in buildings is the release of volatile organic compounds (VOC's). This characteristic was studied at 65 °C by CG-MS. Both samples showed VOC's emission after 10 min of heating, however peaks intensity of VOC's generated from M-2 microcapsules showed a lower concentration than Micronal ® DS 5008 X.

  18. Design and Preparation of Carbon Based Composite Phase Change Material for Energy Piles

    Science.gov (United States)

    Yang, Haibin; Memon, Shazim Ali; Bao, Xiaohua; Cui, Hongzhi; Li, Dongxu

    2017-01-01

    Energy piles—A fairly new renewable energy concept—Use a ground heat exchanger (GHE) in the foundation piles to supply heating and cooling loads to the supported building. Applying phase change materials (PCMs) to piles can help in maintaining a stable temperature within the piles and can then influence the axial load acting on the piles. In this study, two kinds of carbon-based composite PCMs (expanded graphite-based PCM and graphite nanoplatelet-based PCM) were prepared by vacuum impregnation for potential application in energy piles. Thereafter, a systematic study was performed and different characterization tests were carried out on two composite PCMs. The composite PCMs retained up to 93.1% of paraffin and were chemically compatible, thermally stable and reliable. The latent heat of the composite PCM was up to 152.8 J/g while the compressive strength of cement paste containing 10 wt % GNP-PCM was found to be 37 MPa. Hence, the developed composite PCM has potential for thermal energy storage applications. PMID:28772752

  19. Preparation and Characterization of Microencapsulated Phase Change Materials for Use in Building Applications

    Directory of Open Access Journals (Sweden)

    Jessica Giro-Paloma

    2015-12-01

    Full Text Available A method for preparing and characterizing microencapsulated phase change materials (MPCM was developed. A comparison with a commercial MPCM is also presented. Both MPCM contained paraffin wax as PCM with acrylic shell. The melting temperature of the PCM was around 21 °C, suitable for building applications. The M-2 (our laboratory made sample and Micronal® DS 5008 X (BASF samples were characterized using SEM, DSC, nano-indentation technique, and Gas Chromatography/Mass spectrometry (GC-MS. Both samples presented a 6 μm average size and a spherical shape. Thermal energy storage (TES capacities were 111.73 J·g−1 and 99.3 J·g−1 for M-2 and Micronal® DS 5008 X, respectively. Mechanical characterization of the samples was performed by nano-indentation technique in order to determine the elastic modulus (E, load at maximum displacement (Pm, and displacement at maximum load (hm, concluding that M-2 presented slightly better mechanical properties. Finally, an important parameter for considering use in buildings is the release of volatile organic compounds (VOC’s. This characteristic was studied at 65 °C by CG-MS. Both samples showed VOC’s emission after 10 min of heating, however peaks intensity of VOC’s generated from M-2 microcapsules showed a lower concentration than Micronal® DS 5008 X.

  20. Phase change Materials (PCM) microcapsules with different shell compositions: Preparation, characterization and thermal stability

    Energy Technology Data Exchange (ETDEWEB)

    Bayes-Garcia, L.; Ventola, L.; Cordobilla, R.; Benages, R.; Calvet, T.; Cuevas-Diarte, M.A. [Departament de Cristal.lografia, Mineralogia i Diposits Minerals, Facultat de Geologia, Universitat de Barcelona, Marti i Franques s/n, E-08028 Barcelona (Spain)

    2010-07-15

    In this study, phase change materials (Rubitherm registered RT 27) microcapsules were successfully obtained by two different methods. The main difference between them remains on the shell composition, as they are composed of different coacervates (Sterilized Gelatine/Arabic Gum for the SG/AG method and Agar-Agar/Arabic Gum for the AA/AG method). Microcapsules were thermally characterized by thermo-optical microscopy and differential scanning calorimetry. Using scanning electron microscopy, their spherical morphology (sphericity factor of 0.94-0.95) and their particle size distribution were determined, obtaining an average diameter of 12 {mu}m for the SG/AG method and lower values for the AA/AG method, where nanocapsules were also observed (average diameter of 4.3 {mu}m for the microcapsules and 104 nm for the nanocapsules). The thermal stability determination was carried out by Thermogravimetric analyses (TG) and the results show a high decomposition temperature, although the process takes places in four steps for the two mentioned methods. Moreover, the microcapsules obtained by the AA/AG method decompose in a more gradual way, as in the TG results a double step, instead of one, is appreciable. On the whole, the prepared microencapsulated PCM are totally capable of developing their role in thermal energy storage. (author)

  1. Preparation and characterization of form-stable paraffin/polyurethane composites as phase change materials for thermal energy storage

    International Nuclear Information System (INIS)

    Chen, Keping; Yu, Xuejiang; Tian, Chunrong; Wang, Jianhua

    2014-01-01

    Highlights: • Paraffin/polyurethane composite as form-stable phase change material was prepared by bulk polymerization. • Paraffin/polyurethane composite possesses typical character of dual phase transition. • Total latent heat of n-eicosane/PUPCM is as high as 141.2 J/g. • Maximum encapsulation ratio for n-octadecane/PUPCM composites is 25% w/w. - Abstract: Polyurethane phase change material (PUPCM) has been demonstrated to be effective solid–solid phase change material for thermal energy storage. However, the high cost and complex process on preparation of PUPCMs with high enthalpy and broad phase transition temperature range can prohibit industrial-scale applications. In this work, a series of novel form-stable paraffin/PUPCMs composites (n-octadecane/PUPCM, n-eicosane/PUPCM and paraffin wax/PUPCM) with high enthalpy and broad phase transition temperature range (20–65 °C) were directly synthesized via bulk polymerization. The composites were prepared at different mass fractions of n-octadecane (10, 20, 25, 30% w/w). The results indicated that the maximum encapsulation ratio for n-octadecane/PUPCM10000 composites was around 25% w/w. The chemical structure and crystalline properties of these composites were characterized by Fourier transform infrared spectroscopy (FT-IR), polarizing optical microscopy (POM), wide-angle X-ray diffraction (WAXD). Thermal properties and thermal reliability of the composites were determined using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). From DSC analysis, the composites showed a typical dual phase change temperature. The enthalpy for the composite with 25% w/w n-eicosane was as high as 141.2 J/g. TGA analysis indicated that the composites degraded at considerably high temperatures. The process of preparation of PUPCMs and their composites was very simple, inexpensive, environmental friendly and easy to process into desired shapes, which could find the promising applications in solar

  2. Effect of Preparation Method on Phase Formation Process and Structural and Magnetic Properties of Mn2.5Ge Samples

    Directory of Open Access Journals (Sweden)

    R. Sobhani

    2016-12-01

    Full Text Available In this paper, the phase formation process of Mn2.5Ge samples, prepared by mechanical alloying of Mn and Ge metal powders and annealing, has been studied. Results showed that in the milled samples the stable phase is Mn11Ge8 compound with orthorhombic structure and Pnam space group. The value of saturation magnetization increases by increasing milling time from 0.2 up to 1.95 (Am2Kg-1. The remanece of the samples increases by increasing the milling time while the coercivity decreases. Annealing of 15-hour milled sample results in disappearance of Mn and Ge and the formation of new phases of Mn3Ge, Mn5Ge2, Mn5Ge3 and Mn2.3Ge. Mn3Ge is the main phase with Do22 tetragonal structure and I4/mmm space group which is stable and dominant. The enhancement of saturation magnetization in the annealed sample is related to the formation of three new magnetic phases and the increase of coercivity is due to the presence of Mn3Ge compound with tetragonal structure. Studies were replicated on samples made by arc melting method to compare the results and to investigate the effect of the preparation method on phase formation and structural and magnetic properties of the materials. In these samples the saturation value was in range of 0.2 up to 1.95 (Am2Kg-1 depending on preparation methods. Rietveld refinement shows that Mn2.3Ge sample prepared from arc melted under 620oC anealing is single phase. Magnetic analysis of this sample show a saturation magnetization of 5.252(Am2Kg-1 and 0.005 T coercive field.

  3. High mobility In2O3:H transparent conductive oxides prepared by atomic layer deposition and solid phase crystallization

    NARCIS (Netherlands)

    Macco, B.; Wu, Y.; Vanhemel, D.; Kessels, W.M.M.

    2014-01-01

    The preparation of high-quality In2O3:H, as transparent conductive oxide (TCO), is demonstrated at low temperatures. Amorphous In2O3:H films were deposited by atomic layer deposition at 100 °C, after which they underwent solid phase crystallization by a short anneal at 200 °C. TEM analysis has shown

  4. Preparation, characterization, and thermal properties of starch microencapsulated fatty acids as phase change materials thermal energy storage applications

    Science.gov (United States)

    Stable starch-oil composites can be prepared from renewable resources by excess steam jet-cooking aqueous slurries of starch and vegetable oils or other hydrophobic materials. Fatty acids such as stearic acid are promising phase change materials (PCMs) for latent heat thermal energy storage applica...

  5. Preparation of multishell ICF target plastic-foam cushion materials by thermally induced phase-inversion processes

    International Nuclear Information System (INIS)

    Young, A.T.; Moreno, D.K.; Marsters, R.G.

    1981-01-01

    Homogenous, low-density plastic foams for ICF targets have been prepared by thermally induced phase inversion processes. Uniform, open cell foams have been obtained by the rapid freezing of water solutions of modified cellulose polymers with densities in the range of 5 mg/cm 3 to 0.7 mg/cm 3 and respective average cell sizes of 2 to 40 micrometers. In addition, low-density, microcellular foams have been prepared from the hydrocarbon polymer poly(4-methyl-l-pentene) via a similar phase inversion process using homogenous solutions in organic solvents. These foams have densities from 2 to 5 mg/cm 3 and average cell sizes of 20 micrometers. The physical-chemical aspects of the thermally induced phase inversion process is presented

  6. Preparation of CdS microtrumpets from a solvent extraction system by a two-phase approach

    International Nuclear Information System (INIS)

    Geng, Aifang; Liu, Yubing; Liao, Wuping

    2011-01-01

    Highlights: → CdS microtrumpets were prepared from an extraction system by a two-phase approach. → Triethanolamine plays a crucial role in the formation of the trumpets. → Some micro-lotus seedpods can also be obtained with trihydroxymethyl aminomethane. -- Abstract: CdS microtrumpets with the length being of about 4 μm and the bell wall being of 100 nm have been prepared using a cadmium di-(2-ethylhexyl) phosphoric acid chelate as the precursor by a two-phase thermal approach. The products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and UV-vis spectroscopy. The effects of temperature, reaction time, and co-surfactant on the morphology were also examined. It was found that the co-surfactant triethanolamine plays a crucial role in the formation of the cubic phase trumpet-like CdS microstructures.

  7. Preparation and Characterization of HDPE/EVA Flat Sheet Membranes by Thermally Induced Phase Separation Method

    Directory of Open Access Journals (Sweden)

    Zahra Shoeyb

    2015-06-01

    Full Text Available The adjustment of material composition in fabrication of modified polymeric membrane has been considered the most efficient and easiest method. For this purpose blended membranes of high density polyethylene (HDPE–ethylene vinyl acetate (EVA were prepared by thermally induced phase separation method. The impact of EVA in the presence of diluent on the crystalization temperature was assessed using differential scanning calorimetry (DSC. The obtained results showed that EVA has no significant effect on the crystalization temperature of HDPE. The absorption frequencies at 1248 and 1749 cm-1, respectively, due to C-O and C=O streching vibrations of EVA functional groups, confirmed the existence of EVA in HDPE membrane. The pure water permeability of HDPE/EVA blend was measured and compared with that of neat HDPE membrane. The results showed that an EVA content up to 2.5 wt% raised water permeability considerably and the leafy structure of the membranes contracted and the pure water permeation dropped with higher EVA content. The results of porosity measurement and scanning electronic microscopic (SEM analysis also confirmed these findings. Contact angel measurements and atomic force microscopy (AFM examinations and static absorption of collagen protein on the membrane surfaces revealed that EVA content up to 5 wt% lowered the hydrophobicity of the membrane. By EVA content above 10 wt%, due to the structural alteration on the membrane surface, the contact angel and the collagen absorption on the surface of membrane increased. The measurement of tensile strength showed that with increasing EVA content the mechanical properties of the membranes improved due to interactions of polar groups in EVA.

  8. The corrosion mechanism of the sintered (Ce, Nd)-Fe-B magnets prepared by double main phase and single main phase approaches

    Science.gov (United States)

    Shi, Xiaoning; Zhu, Minggang; Zhou, Dong; Song, Liwei; Guo, Zhaohui; Li, Jia; Li, Wei

    2018-05-01

    The sintered (Ce, Nd)-Fe-B magnets were produced widely by Double Main Phase (DMP) method in China as the magnetic properties of the DMP magnets are superior to those of single main phase (SMP) magnets with the same nominal composition. In this work, the microstructure and corrosion mechanism of the sintered (Ce0.2Nd0.8)30FebalB (wt.%) magnets prepared by DMP and SMP method were studied in detail. Compared to SMP magnets, the DMP magnets have more positive corrosion potential, lower corrosion current density, larger electron transfer resistance, and lower mass loss of the free corrosion experiment in 0.5mol/l Na2SO4 aqueous solution. All of the results show that the DMP magnets have better corrosion resistance than SMP magnets. The back scattered electron images show that the crystalline grains of the DMP magnets are sphericity with a smooth surface while the SMP ones have plenty of edges and corners. Besides, the distribution of Ce/Nd is much more uneven in both magnetic phase and rare earth (Re)-rich phase of the DMP magnets than those of SMP magnets. After corrosion, DMP magnets show eroded magnetic phase and intact Re-rich phase, which indicate that galvanic corrosion of the Re-rich phase acting as the cathode appears.

  9. Complexation-Induced Phase Separation: Preparation of Metal-Rich Polymeric Membranes

    KAUST Repository

    Villalobos, Luis Francisco

    2017-01-01

    The majority of state-of-the-art polymeric membranes for industrial or medical applications are fabricated by phase inversion. Complexation induced phase separation (CIPS)—a surprising variation of this well-known process—allows direct fabrication

  10. Preparation and performance of novel polyvinylpyrrolidone/polyethylene glycol phase change materials composite fibers by centrifugal spinning

    Science.gov (United States)

    Zhang, Xiaoguang; Qiao, Jiaxin; Zhao, Hang; Huang, Zhaohui; Liu, Yangai; Fang, Minghao; Wu, Xiaowen; Min, Xin

    2018-01-01

    Currently, phase change materials (PCMs) composite fibers are typically prepared by electrospinning. However, electrospinning exhibits safety concerns and a low production rate, which limit its practical applications as a cost-effective fiber fabrication approach. Therefore, a novel, and simple centrifugal spinning technology is employed to extrude fibers from composite solutions using a high-speed rotary and perforated spinneret. The composite fibers based on polyvinylpyrrolidone (PVP) and polyethylene glycol (PEG) were prepared by centrifugal spinning. The SEM of PVP/PEG composite fibers indicated that the fibrous morphology is well preserved. The DSC and TGA indicated that PVP/PEG composite fibers exhibit good thermal properties.

  11. Characteristic of New Solid-Phase Extraction Sorbent: Activated Carbon Prepared from Rice Husks under Base Treated Condition

    OpenAIRE

    Afrida Kurnia Putri; Wang-Hsien Ding; Han-Wen Kuo

    2012-01-01

    A characterization of activated carbon (ACs) prepared from rice husks (RHs) under base treated condition as a new sorbent for solid-phase extraction (SPE) to extract 4-nonylphenol isomers (4-NPs) in water samples has been done. The ACs prepared from RHs usually exhibits low specific surface area due to its high ash content, but in case of its application for SPE, there are other factors need to be considered, such as the existence of functional groups inside the sorbent, that can enhance inte...

  12. Preparation and Characterization of Silicone Liquid Core/Polymer Shell Microcapsules via Internal Phase Separation

    DEFF Research Database (Denmark)

    Gonzalez, Lidia; Kostrzewska, Malgorzata; Ma, Baoguang

    2014-01-01

    Microcapsules with a silicone liquid core surrounded by a polymeric shell were synthesisedthrough the controlled phase separation. The dispersed silicone phase consisted of the shellpolymer PMMA, a good solvent for the PMMA (dichloromethane, DCM) and a poor solvent(methylhydrosiloxane dimethylsil......Microcapsules with a silicone liquid core surrounded by a polymeric shell were synthesisedthrough the controlled phase separation. The dispersed silicone phase consisted of the shellpolymer PMMA, a good solvent for the PMMA (dichloromethane, DCM) and a poor solvent...

  13. Preparation of Paraffin@Poly(styrene-co-acrylic acid) Phase Change Nanocapsules via Combined Miniemulsion/Emulsion Polymerization.

    Science.gov (United States)

    Zhang, Feng; Liu, Tian-Yu; Hou, Gui-Hua; Guan, Rong-Feng; Zhang, Jun-Hao

    2018-06-01

    The fast development of solid-liquid phase change materials calls for nanomaterials with large specific surface area for rapid heat transfer and encapsulation of phase change materials to prevent potential leakage. Here we report a combined miniemulsion/emulsion polymerization method to prepare poly(styrene-co-acrylic acid)-encapsulated paraffin (paraffin@P(St-co-AA)) nanocapsules. The method could suppress the shortcomings of common miniemulsion polymerization (such as evaporation of monomer and decomposition of initiator during ultrasonication). The paraffin@P(St-co-AA) nanocapsules are uniform in size and the polymer shell can be controlled by the weight ratio of St to paraffin. The phase change behavior of the nanocapsules is similar to that of pure paraffin. We believe our method can also be utilized to synthesize other core-shell phase change materials.

  14. A Phase Transfer Catalyzed Permanganate Oxidation: Preparation of Vanillin from Isoeugenol Acetate.

    Science.gov (United States)

    Lampman, Gary M.; Sharpe, Steven D.

    1983-01-01

    Background information, laboratory procedures, and results are provided for the preparation of vanillin from isoeugenol acetate. Reaction scheme used to prepare the vanillin and a table indicating the different oxidation experiments carried out on isoeugenol or isoeugenol acetate are also provided. (JN)

  15. A method for the preparation of curcumin by ultrasonic-assisted ammonium sulfate/ethanol aqueous two phase extraction.

    Science.gov (United States)

    Xu, Guangkuan; Hao, Changchun; Tian, Suyang; Gao, Feng; Sun, Wenyuan; Sun, Runguang

    2017-01-15

    This study investigated a new and easy-to-industrialized extracting method for curcumin from Curcuma longa rhizomes using ultrasonic extraction technology combined with ammonium sulfate/ethanol aqueous two-phase system (ATPS), and the preparation of curcumin using the semi-preparative HPLC. The single-factor experiments and response surface methodology (RSM) were utilized to determine the optimal material-solvent ratio, ultrasonic intensity (UI) and ultrasonic time. The optimum extraction conditions were finally determined to be material-solvent rate of 3.29:100, ultrasonic intensity of 33.63W/cm 2 and ultrasonic time of 17min. At these optimum conditions, the extraction yield could reach 46.91mg/g. And the extraction yields of curcumin remained stable in the case of amplification, which indicated that scale-up extraction was feasible and efficient. Afterwards, the semi-preparative HPLC experiment was carried out, in which optimal preparation conditions were elected according to the single factor experiment. The prepared curcumin was obtained and the purity could up to 85.58% by the semi-preparative HPLC. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Separation of radioimmunoassay in magnetic phase with particles prepared at the IPEN and its comparison with conventional methodologies

    International Nuclear Information System (INIS)

    Araujo, E.A. de.

    1991-01-01

    In the present work two main objectives were chosen. The first was the preparation for the execution of the magnetic phase separation technique, useful for the radioimmunoassay as well as for the most modern and most efficient immunoradiometric assay. The second objective, of a theoretical-practical kind and directly linked to the first, was the realization of a study about the precision of the technique with synthesized products compared with imported products and with two liquid phase separation techniques: the second antibody and polyethyleneglycol (PEG). This analysis was performed with the help of precision profiles built according to R.P.Ekins' recommendations. (author)

  17. Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.

    Science.gov (United States)

    Wang, Qing; Long, Yao; Yao, Lin; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

    2016-01-01

    A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Phase transformation of aluminium hydroxide to aα- alumina prepared from different aluminium salts

    International Nuclear Information System (INIS)

    Masliana Muslimin; Meor Yusoff Meor Sulaiman

    2006-01-01

    The study intends to look at the most suitable aluminium salt to produce a single-phase a-alumina by the hydrothermal method. In the process to produce alumina from the calcination of aluminium hydroxide (Al(OH) 3 ), three different aluminium salts namely aluminium sulfate (Al 2 (SO 4) 2), aluminium nitrate (A(NO 3 ) 3 ) and aluminium chloride (AlCl 3 ) were tried. The process involved the used of NH 4 OH as the precipitating medium. Aluminium hydroxide produced from each of these salts were characterised by x-ray diffraction (XRD) technique to identity the crystalline phase. Aluminium hydroxide produced by all the different aluminium salts is present as boehmite or pseudo-boehmite phase. Aluminium hydroxide produced from Al 2 (SO) 2 , Al(NO) 3 and AlCl 3 shows the transformation of the boehmite phase to a α-alumina phase at 500 0 C. On further heating, the α-alumina continuously formed at 800 o C followed soon at 1000 o C. But for the Al(NO3) 3 salts a different phase transitions occurs on heating especially at 1000 o C. Here it was observed not a single alumina phase is presence but the presence of both α and γ--alumina phases. At 1300 o C, the single α-alumina phase was formed. The study concluded that aluminium sulphate is recommended in order to obtain a single-phase α-alumina with the required characteristics. (Author)

  19. Easy and industrially applicable impregnation process for preparation of diatomite-based phase change material nanocomposites for thermal energy storage

    International Nuclear Information System (INIS)

    Konuklu, Yeliz; Ersoy, Orkun; Gokce, Ozgur

    2015-01-01

    The high porosity, high oil and water absorption capacity and low density of diatomite make it ideal for industrial applications. The porous structure of diatomite protects phase change materials (PCMs) from environmental factors as a supporting matrix and phase changes occur in nanopores of diatomite. Previous research on diatomite/PCMs composites aimed optimal composite preparation but many methods were feasible only in laboratory scale. In large scale industrial fabrication, easy, continuous and steady state methods are need to be performed. The main purpose of this study was to prepare leakage-free, thermally stable nanocomposite PCMs (nanoCPCMs) by an easy, continuous and steady state method for high temperature thermal energy storage applications. A series of nanoCPCMs with different paraffin:diatomite mass ratios were prepared. The properties of nanoCPCMs have been characterized via scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The leak (exudation) test was performed on prepared composites at higher temperatures (95 °C) in comparison with literature. As the optimum composite for thermal energy storage applications, thermal reliability of nanoCPCM was evaluated after 400 cycles of melting and freezing. NanoCPCM melted at 36.55 °C with latent heat of 53.1 J/g. - Highlights: • Diatomite-based phase change material nanocomposites were prepared. • An easy and industrially applicable impregnation process was developed. • Influence of diatomite: PCM mass ratio on thermal properties reported.

  20. The influence of the thermal regime of the multifilamentary wires preparation to the creation of the Nb3Sn phase

    International Nuclear Information System (INIS)

    Sitek, J.; Hucl, M.; Bajci, P.; Kruzliak, J.; Benacka, S.; Hut'ka, P.; Kovac, P.

    1984-01-01

    On the basis of the results obtained by Moessbauer spectroscopy and by measuring the critical temperature by means of the inductive method, the possibility of creating the Nb 3 Sn phase in the composite filaments CuSn-Nb is discussed. The filaments were prepared by pressing at room temperature, and at temperatures of 550 to 600 deg C. Experimental details are given. Results are given and discussed. (author)

  1. Study of preparation and survey of radioisotopes tracer applications of gold nanoparticles in the multi-phase industrial processes

    International Nuclear Information System (INIS)

    Huynh Thai Kim Ngan; Trinh Cong Son; Duong Thi Bich Chi; Tran Tri Hai; Nguyen Huu Quang; Bui Trong Duy; Le Trong Nghia; Ngo Duc Tin

    2014-01-01

    Gold nanoparticles (AuNPs) were prepared by Turkevich and Brust method. The labeled gold in liquids is the colloidal form with nano size particle of gold. This particles is of high dispersity in the liquid phase that makes them a good physical tracer. The stability and dissolve of AuNPs in solvents such as water, toluene are hereafter discussed. The size of AuNPs was determined through UV-Visible spectroscopy (UV-Vis) and transmission electron microscope (TEM). (author)

  2. Representing Development

    DEFF Research Database (Denmark)

    Representing Development presents the different social representations that have formed the idea of development in Western thinking over the past three centuries. Offering an acute perspective on the current state of developmental science and providing constructive insights into future pathways, ...

  3. Preparation Of Liquid Phase-Double Antibodies Radioimmunoassay For The In Vitro Determination Of Prolactin Hormone In Human Serum

    International Nuclear Information System (INIS)

    MEHANY, N.L.; EL-KOLALY, M.T.; EBEID, N.H.; MEKY, N.H.

    2009-01-01

    In the present study, the preparation of the basic reagents of prolactin (PRL) radioimmunoassay (RIA) technique using liquid phase double antibody with low cost is considered to be the main objective. Three primary components were prepared and characterized to obtain valid and accurate system. These components were polyclonal antibody (anti-PRL), 125 I-prolactin ( 125 I-PRL) radio-iodinated tracer and PRL standards. The production of polyclonal anti-PRL was undertaken by immunizing eight males of white New-Zealand rabbits (two groups) with highly purified PRL antigen through primary injection and five booster doses subcutaneously and intramuscular. The preparation of radio-iodinated ( 1 '2 5 I-PRL) tracer was carried out using chloramine-T method. The preparation of PRL standards were carried out using highly purified PRL antigen in assay buffer. The obtained PRL-antisera were characterized in terms of titer, immuno response and displacement profile. Formulation, optimization and validation of the local liquid phase RIA system were carried out. The results obtained provide a highly sensitive, specific and accurate RIA system of PRL. In conclusion, this technique could be used in diagnosis of pituitary dysfunction such as hyperprolactinaemia and hyperprolactinaemia, prolactinoma, galactorrhoea, amenorrhea and diagnosis of infertility in males and females.

  4. Preparation of high-pressure phase boron nitride films by physical vapor deposition

    CERN Document Server

    Zhu, P W; Zhao, Y N; Li, D M; Liu, H W; Zou Guang Tian

    2002-01-01

    The high-pressure phases boron nitride films together with cubic, wurtzic, and explosive high-pressure phases, were successfully deposited on the metal alloy substrates by tuned substrate radio frequency magnetron sputtering. The percentage of cubic boron nitride phase in the film was about 50% as calculated by Fourier transform infrared measurements. Infrared peak position of cubic boron nitride at 1006.3 cm sup - sup 1 , which is close to the stressless state, indicates that the film has very low internal stress. Transition electron microscope micrograph shows that pure cubic boron nitride phase exits on the surface of the film. The growth mechanism of the BN films was also discussed.

  5. Robotic, MEMS-based Multi Utility Sample Preparation Instrument for ISS Biological Workstation, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — This project will develop a multi-functional, automated sample preparation instrument for biological wet-lab workstations on the ISS. The instrument is based on a...

  6. Universal Sample Preparation Module for Molecular Analysis in Space, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Lynntech proposes to develop and demonstrate the ability of a compact, light-weight, and automated universal sample preparation module (USPM) to process samples from...

  7. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    OpenAIRE

    Helena Prosen

    2014-01-01

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several...

  8. Creating Drug Solubilization Compartments via Phase Separation in Multicomponent Buccal Patches Prepared by Direct Hot Melt Extrusion-Injection Molding.

    Science.gov (United States)

    Alhijjaj, Muqdad; Bouman, Jacob; Wellner, Nikolaus; Belton, Peter; Qi, Sheng

    2015-12-07

    Creating in situ phase separation in solid dispersion based formulations to allow enhanced functionality of the dosage form, such as improving dissolution of poorly soluble model drug as well as being mucoadhesive, can significantly maximize the in vitro and in vivo performance of the dosage form. This formulation strategy can benefit a wide range of solid dosage forms for oral and alternative routes of delivery. This study using buccal patches as an example created separated phases in situ of the buccal patches by selecting the excipients with different miscibility with each other and the model drug. The quaternary dispersion based buccal patches containing PEG, PEO, Tween 80, and felodipine were prepared by direct hot melt extrusion-injection molding (HME-IM). The partial miscibility between Tween 80 and semicrystalline PEG-PEO led to the phase separation after extrusion. The Tween phases acted as drug solubilization compartments, and the PEG-PEO phase had the primary function of providing mucoadhesion and carrier controlled dissolution. As felodipine was preferably solubilized in the amorphous regions of PEG-PEO, the high crystallinity of PEG-PEO resulted in an overall low drug solubilizing capacity. Tween 80 was added to improve the solubilization capacity of the system as the model drug showed good solubility in Tween. Increasing the drug loading led to the supersaturation of drug in Tween compartments and crystalline drug dispersed in PEG-PEO phases. The spatial distribution of these phase-separated compartments was mapped using X-ray micro-CT, which revealed that the domain size and heterogeneity of the phase separation increased with increasing the drug loading. The outcome of this study provides new insights into the applicability of in situ formed phase separation as a formulation strategy for the delivery of poorly soluble drugs and demonstrated the basic principle of excipient selection for such technology.

  9. Preparation, characterization and thermal properties of nanocapsules containing phase change material n-dodecanol by miniemulsion polymerization with polymerizable emulsifier

    International Nuclear Information System (INIS)

    Chen, Zhong-Hua; Yu, Fei; Zeng, Xing-Rong; Zhang, Zheng-Guo

    2012-01-01

    Highlights: ► We prepare nanocapsules containing n-dodecanol via miniemulsion polymerization. ► Polymerizable emulsifier plays important role in the preparation of nanocapsules. ► Adding co-emulsifier into water phase is helpful to encapsulate n-dodecanol. ► The phase change latent heat of nanocapsule is 98.8 J/g with temperature of 18.2 °C. -- Abstract: Nanocapsules containing phase change material (PCM) n-dodecanol as core and polymethyl methacrylate (PMMA) as shell were synthesized by miniemulsion polymerization with polymerizable emulsifier DNS-86 and co-emulsifier hexadecane (HD). The nanocapsules were characterized by using Fourier transform infrared spectroscopy (FTIR), transmission electron microscope (TEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and laser particle diameter analyzer. The effects of polymerizable emulsifier and co-emulsifier on the properties of nanocapsules were studied. The results show that thermal properties of nanocapsules are affected greatly by the addition methods of HD and the amounts of DNS-86 and HD. Adding HD into water phase is helpful for the encapsulation of n-dodecanol. When the mass ratios of DNS-86 to n-dodecanol and the mass ratios of HD to n-dodecanol were 3% and 2%, the phase change latent heat and the encapsulation efficiency of nanocapsules reached to the maximum value of 98.8 J/g and 82.2%, respectively. Spherical nanocapsules with mean diameter of 150 nm and phase change temperature of 18.2 °C are obtained, which are sure to have a good potential for energy storage.

  10. Main corrective measures in an early phase of nuclear power plants’ preparation for safe long term operation

    Energy Technology Data Exchange (ETDEWEB)

    Krivanek, Robert, E-mail: r.krivanek@iaea.org [International Atomic Energy Agency (IAEA), Department of Nuclear Safety and Security, Operational Safety Section, Vienna 1400 (Austria); Fiedler, Jan, E-mail: fiedler@fme.vutbr.cz [University of Technology Brno, Faculty of Mechanical Engineering, Energy Institute, Technická 2896/2, 616 69 Brno (Czech Republic)

    2017-05-15

    Highlights: • Results of SALTO missions provide the most important issues for safe long term operation (LTO) of nuclear power plants. • The most important technical corrective measures in an early phase of preparation for safe LTO are described. • Their satisfactory resolution creates a basis for further activities to demonstrate preparedness for safe LTO. - Abstract: This paper presents the analysis of main technical deficiencies of nuclear power plants (NPPs) in preparedness for safe long term operation (LTO) and the main corrective measures in an early phase of preparation for safe LTO of NPPs. It focuses on technical aspects connected with management of physical ageing of NPP structures, systems and components (SSCs). It uses as a basis results of IAEA SALTO missions performed between 2005 and 2016 (see also paper NED8805 in Nuclear Engineering and Design in May 2016) and the personal experiences of the authors with preparation of NPPs for safe LTO. This paper does not discuss other important aspects of safe LTO of NPPs, e.g. national nuclear energy policies, compliance of NPPs with the latest international requirements on design, obsolescence, environmental impact and economic aspects of LTO. Chapter 1 provides a brief introduction of the current status of the NPP’ fleet in connection with LTO. Chapter 2 provides an overview of SALTO peer review service results with a focus on deficiencies related to physical ageing of safety SSCs and a demonstration that SSCs will perform their safety function during the intended period of LTO. Chapter 3 discusses the main corrective measures which NPPs typically face during the preparation for demonstration of safe LTO. Chapter 4 summarizes the current status of the NPP’ fleet in connection with LTO and outlines further steps needed in preparation for safe LTO.

  11. Integrated Automation of High-Throughput Screening and Reverse Phase Protein Array Sample Preparation

    DEFF Research Database (Denmark)

    Pedersen, Marlene Lemvig; Block, Ines; List, Markus

    into automated robotic high-throughput screens, which allows subsequent protein quantification. In this integrated solution, samples are directly forwarded to automated cell lysate preparation and preparation of dilution series, including reformatting to a protein spotter-compatible format after the high......-throughput screening. Tracking of huge sample numbers and data analysis from a high-content screen to RPPAs is accomplished via MIRACLE, a custom made software suite developed by us. To this end, we demonstrate that the RPPAs generated in this manner deliver reliable protein readouts and that GAPDH and TFR levels can...

  12. Representing dispositions

    Directory of Open Access Journals (Sweden)

    Röhl Johannes

    2011-08-01

    Full Text Available Abstract Dispositions and tendencies feature significantly in the biomedical domain and therefore in representations of knowledge of that domain. They are not only important for specific applications like an infectious disease ontology, but also as part of a general strategy for modelling knowledge about molecular interactions. But the task of representing dispositions in some formal ontological systems is fraught with several problems, which are partly due to the fact that Description Logics can only deal well with binary relations. The paper will discuss some of the results of the philosophical debate about dispositions, in order to see whether the formal relations needed to represent dispositions can be broken down to binary relations. Finally, we will discuss problems arising from the possibility of the absence of realizations, of multi-track or multi-trigger dispositions and offer suggestions on how to deal with them.

  13. Representing time

    Directory of Open Access Journals (Sweden)

    Luca Poncellini

    2010-06-01

    Full Text Available The analysis of natural phenomena applied to architectural planning and design is facing the most fascinating and elusive of the four dimensions through which man attempts to define life within the universe: time. We all know what time is, said St. Augustine, but nobody knows how to describe it. Within architectural projects and representations, time rarely appears in explicit form. This paper presents the results of a research conducted by students of NABA and of the Polytechnic of Milan with the purpose of representing time considered as a key element within architectural projects. Student investigated new approaches and methodologies to represent time using the two-dimensional support of a sheet of paper.

  14. Preparation, characterization and thermal properties of binary nitrate salts/expanded graphite as composite phase change material

    Energy Technology Data Exchange (ETDEWEB)

    Xiao, Junbing [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Huang, Jin, E-mail: huangjiner@126.com [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Zhu, Panpan; Wang, Changhong [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Li, Xinxi [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Center for Nanochemistry, Beijing National Laboratory for Molecular Sciences, State Key Laboratory for Structural Chemistry of Unstable and Stable Species, College of Chemistry and Molecular Engineering, Peking University, Beijing (China)

    2014-07-01

    Highlights: • The expanded graphite enhanced thermal conductivity coefficient greatly. • The aqueous solution method adopting ultrasonic was utilized to disperse EG. • The combination of composite was physical without chemical reaction. • The reduction on total latent heat was slight after the adding EG. - Abstract: The binary nitrate salts/expanded graphite (EG) composite phase change material (PCM) were prepared via adding different mass rate of EG to binary nitrate salts consisting of NaNO{sub 3} and KNO{sub 3} (6:4) by aqueous solution method adopting ultrasonic. The morphology and chemical composition of EG and the composite PCM were characterized and investigated by X-ray diffraction (XRD), scan electron microscope (SEM), energy dispersive spectrometer (EDS), transmission electron microscope (TEM), respectively. Laser thermal conductivity instrument and differential scanning calorimeter (DSC) were employed to measure thermo physical properties. Drawing the conclusion from investigation, that EG had enhanced thermal conductivity coefficient which largely increased to 4.884 W/(m K) and reduced total latent heat by mostly 11.0%. The morphology and phase structure results indicated that EG were well dispersed into and physically combined with molten salts. In general, the prepared composite PCM could be a suitable phase change material for thermal energy storage.

  15. Preparation, characterization and thermal properties of binary nitrate salts/expanded graphite as composite phase change material

    International Nuclear Information System (INIS)

    Xiao, Junbing; Huang, Jin; Zhu, Panpan; Wang, Changhong; Li, Xinxi

    2014-01-01

    Highlights: • The expanded graphite enhanced thermal conductivity coefficient greatly. • The aqueous solution method adopting ultrasonic was utilized to disperse EG. • The combination of composite was physical without chemical reaction. • The reduction on total latent heat was slight after the adding EG. - Abstract: The binary nitrate salts/expanded graphite (EG) composite phase change material (PCM) were prepared via adding different mass rate of EG to binary nitrate salts consisting of NaNO 3 and KNO 3 (6:4) by aqueous solution method adopting ultrasonic. The morphology and chemical composition of EG and the composite PCM were characterized and investigated by X-ray diffraction (XRD), scan electron microscope (SEM), energy dispersive spectrometer (EDS), transmission electron microscope (TEM), respectively. Laser thermal conductivity instrument and differential scanning calorimeter (DSC) were employed to measure thermo physical properties. Drawing the conclusion from investigation, that EG had enhanced thermal conductivity coefficient which largely increased to 4.884 W/(m K) and reduced total latent heat by mostly 11.0%. The morphology and phase structure results indicated that EG were well dispersed into and physically combined with molten salts. In general, the prepared composite PCM could be a suitable phase change material for thermal energy storage

  16. Preparation and characterization of nano-sized phase change emulsions as thermal energy storage and transport media

    International Nuclear Information System (INIS)

    Chen, J.; Zhang, P.

    2017-01-01

    Highlights: • The nano-sized phase change emulsions are prepared by using D-phase method. • The thermo-physical and transport properties are experimentally investigated. • The influence of surfactant on the melting temperature and latent heat of water is clarified. • The phase change emulsion can be used as the heat transfer fluid in a thermal energy storage system. - Abstract: Phase change emulsion (PCE) is a kind of two-phase heat transfer fluid with phase change material (PCM) dispersed in carrier fluid. It has received intensive attractions in recent years due to the fact that it can be used as both the thermal energy storage material and transport medium simultaneously in a thermal energy storage system. In the present study, nano-sized PCEs are prepared by the D-phase method with n-hexadecane and n-octadecane as PCMs. The thermo-physical and transport properties are characterized to facilitate the applications. The droplet size distribution of the PCE is measured by a Photon Correlation Spectroscopy, and the results show that the droplet size distributions are similar at different mass fractions. The rheological behavior and viscosity of the PCE are measured by a rheometer, which shows that the PCEs at mass fractions below 30.0 wt% are Newtonian fluids, and the viscosities are dependent on both the mass fraction and temperature. The differential scanning calorimetry (DSC) is employed to analyze the phase change characteristics of the PCE, and the results indicate large supercooling degree of water and PCM in the PCE. The melting temperature and latent heat of water in the PCE are much smaller than those of pure water. The thermal conductivities of the PCE with different mass fractions at different temperatures are measured by the transient hot-wire method. Furthermore, the energy transport characteristics of the PCEs are evaluated on the basis of the measured thermo-physical and transport properties. The results suggest that the PCEs show a drastic

  17. Bonding and orientation of 1,4-benzenedimethanethiol on Au(111) prepared from solution and from gas phase

    International Nuclear Information System (INIS)

    Pasquali, L; Terzi, F; Zanardi, C; Seeber, R; Paolicelli, G; Mahne, N; Nannarone, S

    2007-01-01

    The orientation and bonding of 1,4-benzenedimethanethiol molecules on Au(111) is studied by means of x-ray and ultraviolet (UV) photoemission, x-ray absorption and metastable deexcitation spectroscopy. The organic films are prepared both from solution and by exposing the clean substrate to the vapours of the substance in an evacuated environment. This leads to two different growth modes: when self-assembled monolayers (SAMs) are prepared from solution, the molecules tend to form a bilayer film with the molecules standing upright and with the molecular axis forming an angle of about 30 0 with respect to the substrate normal; when growth is carried out from the gas phase, the molecules tend to assume at the earliest stages of exposure a flat-lying configuration, with both sulfur end-groups bonding to Au; at increasing exposure the surface coverage presents a saturation and the chemisorbed molecules tend to assume an upright arrangement

  18. Indium tin oxide thin-films prepared by vapor phase pyrolysis for efficient silicon based solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Simashkevich, Alexei, E-mail: alexeisimashkevich@hotmail.com [Institute of Applied Physics, 5 Academiei str., Chisinau, MD-2028, Republic of Moldova (Moldova, Republic of); Serban, Dormidont; Bruc, Leonid; Curmei, Nicolai [Institute of Applied Physics, 5 Academiei str., Chisinau, MD-2028, Republic of Moldova (Moldova, Republic of); Hinrichs, Volker [Institut für Heterogene Materialsysteme, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Lise-Meitner Campus, Hahn-Meitner-Platz 1, 14109 Berlin (Germany); Rusu, Marin [Institute of Applied Physics, 5 Academiei str., Chisinau, MD-2028, Republic of Moldova (Moldova, Republic of); Institut für Heterogene Materialsysteme, Helmholtz-Zentrum Berlin für Materialien und Energie GmbH, Lise-Meitner Campus, Hahn-Meitner-Platz 1, 14109 Berlin (Germany)

    2016-07-01

    The vapor phase pyrolysis deposition method was developed for the preparation of indium tin oxide (ITO) thin films with thicknesses ranging between 300 and 400 nm with the sheet resistance of 10–15 Ω/sq. and the transparency in the visible region of the spectrum over 80%. The layers were deposited on the (100) surface of the n-type silicon wafers with the charge carriers concentration of ~ 10{sup 15} cm{sup −3}. The morphology of the ITO layers deposited on Si wafers with different surface morphologies, e.g., smooth (polished), rough (irregularly structured) and textured (by inversed pyramids) was investigated. The as-deposited ITO thin films consist of crystalline columns with the height of 300–400 nm and the width of 50–100 nm. Photovoltaic parameters of mono- and bifacial solar cells of Cu/ITO/SiO{sub 2}/n–n{sup +} Si/Cu prepared on Si (100) wafers with different surface structures were studied and compared. A maximum efficiency of 15.8% was achieved on monofacial solar cell devices with the textured Si surface. Bifacial photovoltaic devices from 100 μm thick Si wafers with the smooth surface have demonstrated efficiencies of 13.0% at frontal illumination and 10% at rear illumination. - Highlights: • ITO thin films prepared by vapor phase pyrolysis on Si (100) wafers with a smooth (polished), rough (irregularly structured) and textured (by inversed pyramids) surface. • Monofacial ITO/SiO2/n-n+Si solar cells with an efficiency of 15.8% prepared and bifacial PV devices with front- and rear-side efficiencies up to 13% demonstrated. • Comparative studies of photovoltaic properties of solar cells with different morphologies of the Si wafer surface presented.

  19. Solid Phase Radioimmunoassay for Measuring Serum Triiodothyronine and Thyroxine using Different Preparations of Their Labeled Hormones

    International Nuclear Information System (INIS)

    El Kolaly, M.T; Mehany, N.L; Ayyoub, S.M.; Hassan, S.E.M.

    2005-01-01

    The goal of the present work was oriented to prepare stable polystyrene coated tubes for direct radioimmunoassay (RIA) of triiodothyronine (T 3 ) and thyroxine (T 4 ) in human serum or plasma. Coating process was performed using sheep polyclonal antisera specific for each of T 3 and T 4 . The stability study showed that these tubes could be stored for up to one year at 4 degree without any appreciable reduction in their binding. The preparations of 25 I-T 3 and 125 I-T 4 were carried out by two different methods [chloramine-T(Ch-T) and iodogen] . It was found that Ch-T method gave approximately the same results as iodogen method. Twenty five samples of different thyroid status were assayed for T 3 and T 4 using the present systems and with commerically available kits (coated tubes, DPC). The statistical analysis revealed good correlations between the results from the present systems using T 3 and T 4 tracers prepared by Ch-T and iodogen methods and The DPC kits. This may be extremely helpful in diagnosis and proper management of thyroid dysfunctions

  20. Preparation of {sup 183,184}Re samples for modelling a rapid gas phase chemistry of Nielsbohrium (Ns), element 107

    Energy Technology Data Exchange (ETDEWEB)

    Eichler, R.; Gaeggeler, H.W.; Eichler, B.; Tuerler, A. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    Chemical gas phase reactions of the heavier group 7 elements in the system O{sub 2}/H{sub 2}O are presumably best suited for a separation of Nielsbohrium from the lighter transactinides. We expect a higher reaction velocity using the more reactive gas system O{sub 3}/H{sub 2}O{sub 2}. For the experimental verification of this idea we prepared {sup 183}Re/{sup 184}Re samples for thermochromatography experiments with both gas systems. (author) 8 refs.

  1. Fe-Zn intermetallic phases prepared by diffusion annealing and spark-plasma sintering

    Czech Academy of Sciences Publication Activity Database

    Pokorný, P.; Cinert, Jakub; Pala, Zdeněk

    2016-01-01

    Roč. 50, č. 2 (2016), s. 253-256 ISSN 1580-2949 R&D Projects: GA ČR GB14-36566G Institutional support: RVO:61389021 Keywords : Fe-Zn intermetallics * spark-plasma sintering * diffusion annealing * phase composition * hardness Subject RIV: JK - Corrosion ; Surface Treatment of Materials Impact factor: 0.436, year: 2016

  2. Preparation and characterization of form-stable paraffin/polycaprolactone composites as phase change materials for thermal energy storage

    Directory of Open Access Journals (Sweden)

    Aludin M.S.

    2017-01-01

    Full Text Available Paraffin is Phase Change Materials (PCM that possesses desirable properties such as high thermal energy storage and thermal stability to make it suitable for thermal energy storage applications. However, paraffin has been reported to leak out during the melting process. In this study, composites were prepared by dissolving paraffin and polycaprolactone (PCL at varied mass percent compositions in chloroform and then purified through precipitation techniques. The leakage test was conducted by placing the composite samples on a set of four-layer filter papers and left in a furnace at 90°C for 1 hour. By incorporating PCL into paraffin phase, the leakage mass percentage was drastically reduced. The PCL polymer matrix in the composites may have trapped the paraffin molecules during melting process thus prevent it from leaking.

  3. Study on preparation of montmorillonite-based composite phase change materials and their applications in thermal storage building materials

    International Nuclear Information System (INIS)

    Fang Xiaoming; Zhang Zhengguo; Chen Zhonghua

    2008-01-01

    Three composite phase change materials (PCMs) were prepared by blending butyl stearate, dodecanol and RT20 with an organically modified montmorillonite (MMT), respectively. After the three composite PCMs were characterized by DSC, it was indicated that the RT20/MMT composite PCM was a good candidate for building applications due to its large latent heat, suitable phase change temperature and good performance stability. Compared with RT20, the RT20/MMT composite PCM exhibited higher heat transfer efficiency and had good compatibility with gypsum due to the combination with MMT. The composite gypsum boards containing RT20/MMT composite PCM had the function of reducing building energy consumption by reducing the indoor temperature variation, and the function was enhanced with the increase in the mass ratio of the RT20/MMT composite PCM

  4. The preparation and infrared radar stealth performance test of a new paraffin-based phase transition microcapsule

    Science.gov (United States)

    Chen, Yingming; Zhang, Honghong; Gao, Weiting; Chen, Yingmin; Wang, Yifan

    2018-04-01

    For the problems that the phase change material apply to infrared stealth exists easy to broken, hard to control temperature, narrow infrared channel and based on the basic principles of infrared stealth technology, this paper proposed a scheme of thermal infrared composite invisibility multi-layer wrapping, which based on two sides, one is to control the material surface temperature, another is to reduce its infrared emissivity and combine with visible light pigment and electromagnetic wave absorbing material, to realize the materials' wide band compatible stealth. First, choose urea formaldehyde resin and paraffin to prepare multiphase-change microcapsules, and then combine it with the ferroferric oxide absorbing material, zinc oxide visible light pigment, to make the stealth material of wide band. The experimental results show that the new phase change capsule can realize the function of temperature control and infrared stealth in a special temperature range.

  5. Phase transitions in LiCoO2 thin films prepared by pulsed laser deposition

    International Nuclear Information System (INIS)

    Huang Rong; Hitosugi, Taro; Fisher, Craig A.J.; Ikuhara, Yumi H.; Moriwake, Hiroki; Oki, Hideki; Ikuhara, Yuichi

    2012-01-01

    Highlights: ► Epitaxial LiCoO 2 thin films were formed on the Al 2 O 3 (0 0 0 1) substrate by PLD at room temperature and annealed at 600 °C in air. ► The orientation relationship between film and substrate is revealed. ► Crystalline phases in the RT deposited and annealed thin films are clearly identified. ► Atomic level interface structure indicates an interface reaction during annealing. ► A phase transition mechanism from fully disordered LiCoO 2 to fully ordered LiCoO 2 is proposed. - Abstract: Microstructures of epitaxial LiCoO 2 thin films formed on the (0 0 0 1) surface of sapphire (α-Al 2 O 3 ) substrates by pulsed laser deposition at room temperature and annealed at 600 °C in air were investigated by a combination of selected-area electron diffraction, high-resolution transmission electron microscopy, spherical-aberration-corrected high-angle annular dark-field scanning transmission electron microscopy, and electron energy-loss spectroscopy. As-deposited LiCoO 2 thin films consisted of epitaxial grains of the fully cation-disordered phase (γ) with a cubic rock-salt structure. During annealing, this cubic-structured phase transformed into the fully ordered trigonal (α) phase oriented with its basal plane parallel to the surface of the sapphire substrate. Although overall the film appeared to be a single crystal, a small number of Co 3 O 4 grains were also observed in annealed thin films, indicating that some Li and O had been lost during processing. The atomically sharp interface between the film and substrate also became rougher during annealing, with step defects being formed, suggesting that a localized reaction occurred at the interface.

  6. [Preparation and evaluation of stationary phase of high performance liquid chromatography for the separation of basic solutes].

    Science.gov (United States)

    Wang, P; Wang, J; Cong, R; Dong, B

    1997-05-01

    A bonded phase for high performance liquid chromatography (HPLC) has been prepared by the new reaction between silica and silicon ether. The ether was synthesized from alkylchlorosilane and pentane-2,4-dione in the presence of imidazole under inert conditions by using anhydrous tetrahydrofuran as solvent. The bonded phase thus obtained was characterized by elemental analysis, diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy and HPLC evaluation. The carbon content was 9.4% and the surface coverage almost attained 3.0micromol/m2 without end-capping. The silanol absorption peaks of the product cannot be observed from the DRIFT spectrum, which revealed that the silanization reaction proceeded thoroughly. The basic solutes, such as aniline, o-toluidine, p-toluidine, N,N-dimethylaniline and pyridine were used as the probe solutes to examine their interaction with the residual silanols on the surface of the products. No buffer or salt was used in the mobile phase for these experiments. In comparison with an acidic solute, such as, phenol, basic aniline eluted in front of phenol, and the ratio of asymmetry of aniline peak to that of the phenol peak was 1.1. Furthermore the relative k' value of p-toluidine to that of o-toluidine was also 1.1. All the results showed that the stationary phase has better quality and reproducibility and can be used for the separation of basic solutes efficiently.

  7. Preparation, characterization, and thermal properties of the microencapsulation of a hydrated salt as phase change energy storage materials

    International Nuclear Information System (INIS)

    Huang, Jin; Wang, Tingyu; Zhu, Panpan; Xiao, Junbin

    2013-01-01

    Highlights: ► Phase change point and fusion heat of samples are about 51 °Cand 150 J/g respectively. ► DSC results indicated the core material is not Na 2 HPO 4 ·12H 2 O but Na 2 HPO 4 ·7H 2 O. ► Encapsulation takes a significant role in reducing subcooling degree. - Abstract: Microcapsules loaded by disodium hydrogen phosphate heptahydrate (Na 2 HPO 4 ·7H 2 O) were prepared by means of the suspension copolymerization-solvent volatile method, with modified polymethylmethacrylate (PMMA) as coating polymer under the conditions of various organic solvents. The formation of the microencapsulated phase change materials (MEPCMs)-PMMA/Na 2 HPO 4 ·7H 2 O was investigated and analyzed. The morphology of the resultant materials was characterized by using scanning electron microscope (SEM) and phase contrast microscope. Its final composition was confirmed by the Fourier transformation infrared (FT-IR). Thermo gravimetric analyzer (TGA) and differential scanning calorimetry (DSC) were adopted to reveal its thermal stability and thermal properties. Results indicated that the materials owned improved subcooling degree and good thermal properties, enabling the materials to be one promising phase change materials for thermal energy storage

  8. Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

    Science.gov (United States)

    Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

    2015-05-29

    Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Preparation and mechanical properties of liquid-phase sinterd silicon carbide; Herstellung und mechanische Eigenschaften von fluessigphasengesintertem Siliziumkarbid

    Energy Technology Data Exchange (ETDEWEB)

    Wiedmann, I.

    1998-12-01

    Liquid-phase sintered silicon carbide ceramics, LPS-SiC, were prepared, and the influence of structure and chemical secondary phase composition on the mechanical properties was investigated in order to identify LPS-SiC materials which can be produced reproducibly and with low loss of mass by simple techniques, i.e. without powder bed or encapsulation. Their profile of characteristics should be superior to conventional solid-phase sintered SiC and should be comparable with liquid-phase sintered silicon nitride ceramics. [Deutsch] In der vorliegenden Arbeit wurden fluessigphasengesinterte Siliziumkarbid-Keramiken, LPS-SiC, hergestellt und der Einfluss der Gefuegeausbildung und der chemischen Sekundaerphasenzusammensetzung auf die mechanischen Eigenschaften untersucht. Ziel war es, LPS-SiC-Materialien zu identifizieren, die ohne besonderen Vorkehrungen wie Pulverbett oder Einkapselung reproduzierbar und mit geringem Masseverlust hergestellt werden koennen. Das Eigenschaftsprofil sollte deutlich ueber dem von konventionell festphasengesintertem SiC liegen und vergleichbar zu fluessigphasengesinterten Siliziumnitrid-Keramiken sein. (orig.)

  10. Preparation, characterization, and thermal properties of the microencapsulation of a hydrated salt as phase change energy storage materials

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Jin, E-mail: huangjiner@126.com [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China); Wang, Tingyu; Zhu, Panpan; Xiao, Junbin [School of Materials and Energy, Guangdong University of Technology, 510006 Guangzhou (China)

    2013-04-10

    Highlights: ► Phase change point and fusion heat of samples are about 51 °Cand 150 J/g respectively. ► DSC results indicated the core material is not Na{sub 2}HPO{sub 4}·12H{sub 2}O but Na{sub 2}HPO{sub 4}·7H{sub 2}O. ► Encapsulation takes a significant role in reducing subcooling degree. - Abstract: Microcapsules loaded by disodium hydrogen phosphate heptahydrate (Na{sub 2}HPO{sub 4}·7H{sub 2}O) were prepared by means of the suspension copolymerization-solvent volatile method, with modified polymethylmethacrylate (PMMA) as coating polymer under the conditions of various organic solvents. The formation of the microencapsulated phase change materials (MEPCMs)-PMMA/Na{sub 2}HPO{sub 4}·7H{sub 2}O was investigated and analyzed. The morphology of the resultant materials was characterized by using scanning electron microscope (SEM) and phase contrast microscope. Its final composition was confirmed by the Fourier transformation infrared (FT-IR). Thermo gravimetric analyzer (TGA) and differential scanning calorimetry (DSC) were adopted to reveal its thermal stability and thermal properties. Results indicated that the materials owned improved subcooling degree and good thermal properties, enabling the materials to be one promising phase change materials for thermal energy storage.

  11. Atomic pairwise distribution function analysis of the amorphous phase prepared by different manufacturing routes

    DEFF Research Database (Denmark)

    Boetker, Johan P.; Koradia, Vishal; Rades, Thomas

    2012-01-01

    was subjected to quench cooling thereby creating an amorphous form of the drug from both starting materials. The milled and quench cooled samples were, together with the crystalline starting materials, analyzed with X-ray powder diffraction (XRPD), Raman spectroscopy and atomic pair-wise distribution function...... (PDF) analysis of the XRPD pattern. When compared to XRPD and Raman spectroscopy, the PDF analysis was superior in displaying the difference between the amorphous samples prepared by milling and quench cooling approaches of the two starting materials....

  12. Preparation of n-tetradecane-containing microcapsules with different shell materials by phase separation method

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Rui [Department of Chemical Engineering, Tsinghua University, Beijing (China); Zhang, Yan; Zhang, Qingwu [Department of Chemical Engineering, China University of Mining and Technology, Beijing (China); Wang, Xin; Zhang, Yinping [Department of Building Science, Tsinghua University, Beijing (China)

    2009-10-15

    Microcapsules for thermal energy storage and heat-transfer enhancement have attracted great attention. Microencapsulation of n-tetradecane with different shell materials was carried out by phase separation method in this paper. Acrylonitrile-styrene copolymer (AS), acrylonitrile-styrene-butadiene copolymer (ABS) and polycarbonate (PC) were used as the shell materials. The structures, morphologies and the thermal capacities of the microcapsules were characterized using Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The ternary phase diagrams showed the potential encapsulation capabilities of the three shell materials. The effects of the shell/core ratio and the molecular weight of the shell material on the encapsulation efficiency and the thermal capacity of the microcapsules were also discussed. Microcapsules with melting enthalpy > 100 J/g, encapsulation efficiency 66-75%, particle size<1 {mu}m were obtained for all three shell materials. (author)

  13. Microstructure and phase stability of W-Cr alloy prepared by spark plasma sintering

    Czech Academy of Sciences Publication Activity Database

    Vilémová, Monika; Illková, Ksenia; Lukáč, František; Matějíček, Jiří; Klečka, Jakub; Leitner, J.

    2018-01-01

    Roč. 127, February (2018), s. 173-178 ISSN 0920-3796 R&D Projects: GA ČR(CZ) GA17-23964S Institutional support: RVO:61389021 Keywords : Tungsten-chromium alloy * Phase stability * Decomposition * Thermal conductivity * Self-passivating alloys * Spark plasma sintering Subject RIV: JJ - Other Materials OBOR OECD: Materials engineering Impact factor: 1.319, year: 2016 https://www.sciencedirect.com/science/article/pii/S092037961830005X

  14. Copolymerization preparation of cationic cyclodextrin chiral stationary phases for drug enantioseparation in chromatography

    OpenAIRE

    sprotocols

    2015-01-01

    Authors: Ren-Qi Wang, Teng-Teng Ong, Ke Huang, Weihua Tang & Siu-Choon Ng ### Abstract We described a facile and effective protocol wherein radical copolymerization is employed to covalently bond cationic β-cyclodextrin (β-CD) onto silica particles with extended linkage, resulting in a chiral stationary phase (IMPCSP) that can be used for the enantioseparation of racemic drugs in both high-performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC). Starting ...

  15. Preparative conditions and vibrational study of HUP : phase transition and conductivity mechanisms

    International Nuclear Information System (INIS)

    Thi, M.P.; Novak, A.; Colomban, Ph.

    1985-01-01

    Among solid protonic conductors HUP (H 3 OUO 2 PO 4 .3 H 2 O) exhibits very high conducting properties. Uranyl/phosphate hydrates belonging to the HUP family (HUP ; UO 2 (H 2 PO 4 ) 2 .3 H 2 O ; (U= 2 ) 3 (PO 4 ) 2 .4 H 2 O ; (UO O 2 )sub(1.43)PO 4 Hsub(0.14) 2-3.5 H 2 O) have been synthesized in different forms (crystals, powders, films, ...) and characterized by various methods: chemical analysis, DTA, TGA, SEM, X-Ray diffraction, IR and Raman spectroscopy. Morphological studies reveal the presence of various particulat es, from ultrafine powders ( 2 O washing of HUP. Infrared and Raman spectra of polycrystalline H 3 OUO 2 PO 4 .3 H 2 O (HUP) have been investigated at various temperatures between 50 K and 300 K. The most temperature-sensitive bands correspond to PO 4 and H 2 O librations; U-OPO 3 stretching and OH stretching vibrations indicate four different phases of HUP and allow to propose a phasetransition mechanism from a bidimensionnal, quasi-liquid state of a protonated species in the room-temperature phase to a fully ordered crystal below 130 K. The protonic conductivity mechanism of room- and low-temperature phases is discussed. (author)

  16. Streamlined Membrane Proteome Preparation for Shotgun Proteomics Analysis with Triton X-100 Cloud Point Extraction and Nanodiamond Solid Phase Extraction

    Directory of Open Access Journals (Sweden)

    Minh D. Pham

    2016-05-01

    Full Text Available While mass spectrometry (MS plays a key role in proteomics research, characterization of membrane proteins (MP by MS has been a challenging task because of the presence of a host of interfering chemicals in the hydrophobic protein extraction process, and the low protease digestion efficiency. We report a sample preparation protocol, two-phase separation with Triton X-100, induced by NaCl, with coomassie blue added for visualizing the detergent-rich phase, which streamlines MP preparation for SDS-PAGE analysis of intact MP and shot-gun proteomic analyses. MP solubilized in the detergent-rich milieu were then sequentially extracted and fractionated by surface-oxidized nanodiamond (ND at three pHs. The high MP affinity of ND enabled extensive washes for removal of salts, detergents, lipids, and other impurities to ensure uncompromised ensuing purposes, notably enhanced proteolytic digestion and down-stream mass spectrometric (MS analyses. Starting with a typical membranous cellular lysate fraction harvested with centrifugation/ultracentrifugation, MP purities of 70%, based on number (not weight of proteins identified by MS, was achieved; the weight-based purity can be expected to be much higher.

  17. Cu-Nb3Sn superconducting wires prepared by ''Copper Liquid Phase Sintering method'' using the Nb-H

    International Nuclear Information System (INIS)

    Resende, A.T. de.

    1985-01-01

    Cu-30% Nb in weighting were prepared by the method of Copper sintering liquid phase the method was improved by substitution of Nb power by Nb-H powder, obtaining a high density material with good mechanical properties, which was reduced to fine. Wire, Without heat treatment. The Cu-Nb 3 Sn wires were obtained by external diffusion process depositing tin in the Cu-30%Nb wires, and by internal diffusion process using the Sn-8.5% Cu in weighting, which was reduced to rods of 3.5 mm. These Cu-30%Nb rods were enclosed in copper tubes and deformed mechanically by rotary swaging and drawing. During the drawing step some wires were fractured, that were analysed and correlated with the microstructure of the Sn-8.5 Wt% Cu alloy. External and internal diffusion samples; after a fast thermal treatment for Sn diffusion, were submited to the temperature of 700 0 C to provide the reaction between Sn and Nb, leading to the Nb 3 Sn phase. Samples with several reaction times, and its influence on T c and J c critical parameters and normal resistivity were prepared and analysed. (author) [pt

  18. Preparation of steroid radioligands for ultrafiltration assays by a solid-phase transport globulin method using concanavalin A-Sepharose

    International Nuclear Information System (INIS)

    Hiramatsu, R.; Nisula, B.C.

    1985-01-01

    Concanavalin A-Sepharose (Con A-Sepharose) was applied to separate non-protein-bound and albumin-bound radioactive impurities from steroid radioligands. Con A-Sepharose gel, plasma, and steroid radioligand were mixed, incubated, and then washed with buffer. This method was compared with an affinity diafiltration method which separates non-protein-bound radioactive impurities with a filter membrane. 3 H-Water and 3 H-estrone sulfate, chosen to serve as molecules representative of non-protein-bound and albumin-bound impurities, were removed quite effectively by the Con A-Sepharose method, while 85% of 3 H-estrone sulfate could not be removed by the diafiltration method. Plasma unbound cortisol (F) and testosterone (T) values determined by ultrafiltration using 3 H-F and 3 H-T prepared by the Con A-Sepharose method were significantly lower than those determined using the radioligands unprocessed or prepared by the diafiltration method. The whole procedure of the Con A-Sepharose method takes only 3-4 hours. This method is a simple, rapid, and effective technique for preparation of steroid radioligands for plasma protein binding studies

  19. Preparation, characterization and application of N-methylene phosphonic acid chitosan grafted magnesia–zirconia stationary phase

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Qing; Chen, Jie; Huang, Kun; Zhang, Xin; Xu, Li [Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030 (China); Shi, Zhi-guo, E-mail: shizg@whu.edu.cn [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2015-01-07

    Highlights: • N-methylene phosphonic acid chitosan grafted MgO–ZrO{sub 2} was prepared. • It exhibited superior HILIC chromatographic performance to the bare MgO–ZrO{sub 2}. • Monosaccharides, phospholipids and peptides were successfully separated. • It was a promising HILIC stationary phase. - Abstract: A hydrophilic stationary phase (SP) was prepared through grafting N-methylene phosphonic acid chitosan on magnesia–zirconia particles (P-CTS-MgO–ZrO{sub 2}) via Lewis acid–base interaction. The resulting material was characterized by thermogravimetric analysis, Fourier transform infrared spectroscopy, scanning electron microscope and nitrogen adsorption analysis. The chromatographic performance of P-CTS-MgO–ZrO{sub 2} was systemically evaluated by studying effect of acetonitrile content, pH and buffer concentration in the mobile phase. The results demonstrated that the novel SP provided hydrophilic, electrostatic-repulsion and ion-exchange interactions. Compared to the bare MgO–ZrO{sub 2}, P-CTS-MgO–ZrO{sub 2} exhibited superior peak shape, reasonable resolution and reduced analysis time in separation of basic analytes. Besides, remarkable resolving power of acids, i.e. six non-steroidal anti-inflammatory drugs which failed to be eluted from the bare MgO–ZrO{sub 2}, was obtained with the theoretical plate number (N/m) of 4653–31313, asymmetry factor <1.21 and the resolution of 1.6–3.4. Finally, P-CTS-MgO–ZrO{sub 2} SP was applied to separate monosaccharides, phospholipids and peptides. P-CTS-MgO–ZrO{sub 2} was a promising hydrophilic SP for wide applications.

  20. A novel bio-safe phase separation process for preparing open-pore biodegradable polycaprolactone microparticles.

    Science.gov (United States)

    Salerno, Aurelio; Domingo, Concepción

    2014-09-01

    Open-pore biodegradable microparticles are object of considerable interest for biomedical applications, particularly as cell and drug delivery carriers in tissue engineering and health care treatments. Furthermore, the engineering of microparticles with well definite size distribution and pore architecture by bio-safe fabrication routes is crucial to avoid the use of toxic compounds potentially harmful to cells and biological tissues. To achieve this important issue, in the present study a straightforward and bio-safe approach for fabricating porous biodegradable microparticles with controlled morphological and structural features down to the nanometer scale is developed. In particular, ethyl lactate is used as a non-toxic solvent for polycaprolactone particles fabrication via a thermal induced phase separation technique. The used approach allows achieving open-pore particles with mean particle size in the 150-250 μm range and a 3.5-7.9 m(2)/g specific surface area. Finally, the combination of thermal induced phase separation and porogen leaching techniques is employed for the first time to obtain multi-scaled porous microparticles with large external and internal pore sizes and potential improved characteristics for cell culture and tissue engineering. Samples were characterized to assess their thermal properties, morphology and crystalline structure features and textural properties. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Phase transition and thermal expansion studies of alumina thin films prepared by reactive pulsed laser deposition.

    Science.gov (United States)

    Balakrishnan, G; Thirumurugesan, R; Mohandas, E; Sastikumar, D; Kuppusami, P; Songl, J I

    2014-10-01

    Aluminium oxide (Al2O3) thin films were deposited on Si (100) substrates at an optimized oxygen partial pressure of 3 x 10(-3) mbar at room temperature by pulsed laser deposition (PLD). The films were characterized by high temperature X-ray diffraction (HTXRD), field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). The HTXRD pattern showed the cubic y-Al2O3 phase in the temperature range 300-973 K. At temperatures ≥ 1073 K, the δ and θ-phases of Al2O3 were observed. The mean linear thermal expansion coefficient and volume thermal expansion coefficient of γ-Al2O3 was found to be 12.66 x 10(-6) K(-1) and 38.87 x 10(-6) K(-1) in the temperature range 300 K-1073 K. The field emission scanning electron microscopy revealed a smooth and structureless morphology of the films deposited on Si (100). The atomic force microscopy study indicated the increased crystallinity and surface roughness of the films after annealing at high temperature.

  2. A Dual-Phase Ceramic Membrane with Extremely High H2 Permeation Flux Prepared by Autoseparation of a Ceramic Precursor.

    Science.gov (United States)

    Cheng, Shunfan; Wang, Yanjie; Zhuang, Libin; Xue, Jian; Wei, Yanying; Feldhoff, Armin; Caro, Jürgen; Wang, Haihui

    2016-08-26

    A novel concept for the preparation of multiphase composite ceramics based on demixing of a single ceramic precursor has been developed and used for the synthesis of a dual-phase H2 -permeable ceramic membrane. The precursor BaCe0.5 Fe0.5 O3-δ decomposes on calcination at 1370 °C for 10 h into two thermodynamically stable oxides with perovskite structures: the cerium-rich oxide BaCe0.85 Fe0.15 O3-δ (BCF8515) and the iron-rich oxide BaCe0.15 Fe0.85 O3-δ (BCF1585), 50 mol % each. In the resulting dual-phase material, the orthorhombic perovskite BCF8515 acts as the main proton conductor and the cubic perovskite BCF1585 as the main electron conductor. The dual-phase membrane shows an extremely high H2 permeation flux of 0.76 mL min(-1)  cm(-2) at 950 °C with 1.0 mm thickness. This auto-demixing concept should be applicable to the synthesis of other ionic-electronic conducting ceramics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Complexation-Induced Phase Separation: Preparation of Metal-Rich Polymeric Membranes

    KAUST Repository

    Villalobos Vazquez de la Parra, Luis Francisco

    2017-08-01

    The majority of state-of-the-art polymeric membranes for industrial or medical applications are fabricated by phase inversion. Complexation induced phase separation (CIPS)—a surprising variation of this well-known process—allows direct fabrication of hybrid membranes in existing facilities. In the CIPS process, a first step forms the thin metal-rich selective layer of the membrane, and a succeeding step the porous support. Precipitation of the selective layer takes place in the same solvent used to dissolve the polymer and is induced by a small concentration of metal ions. These ions form metal-coordination-based crosslinks leading to the formation of a solid skin floating on top of the liquid polymer film. A subsequent precipitation in a nonsolvent bath leads to the formation of the porous support structure. Forming the dense layer and porous support by different mechanisms while maintaining the simplicity of a phase inversion process, results in unprecedented control over the final structure of the membrane. The thickness and morphology of the dense layer as well as the porosity of the support can be controlled over a wide range by manipulating simple process parameters. CIPS facilitates control over (i) the thickness of the dense layer throughout several orders of magnitude—from less than 15 nm to more than 6 μm, (ii) the type and amount of metal ions loaded in the dense layer, (iii) the morphology of the membrane surface, and (iv) the porosity and structure of the support. The nature of the CIPS process facilitates a precise loading of a high concentration of metal ions that are located in only the top layer of the membrane. Moreover, these metal ions can be converted—during the membrane fabrication process—to nanoparticles or crystals. This simple method opens up fascinating possibilities for the fabrication of metal-rich polymeric membranes with a new set of properties. This dissertation describes the process in depth and explores promising

  4. Preparation and thermal properties of form stable paraffin phase change material encapsulation

    International Nuclear Information System (INIS)

    Liu Xing; Liu Hongyan; Wang Shujun; Zhang Lu; Cheng Hua

    2006-01-01

    Paraffin waxes are cheap and have moderate thermal energy storage density but low thermal conductivity and, hence, require large surface area to be used in energy storage. Form stable paraffin phase change materials (PCM) in which paraffin serves as a latent heat storage material and polyolefins act as a supporting material, because of paraffin leakage, are required to be improved. The form stable paraffin PCM in the present paper was encapsulated in an inorganic silica gel polymer successfully by in situ polymerization. The differential scanning calorimeter (DSC) was used to measure its thermal properties. At the same time, the Washburn equation, which measures the wetting properties of powder materials, was used to test the hydrophilic-lipophilic properties of the PCMs. The result indicated that the enthalpy of the microencapsulated PCMs was reduced little, while their hydrophilic properties were enhanced largely

  5. Preparation of manganese doped cadmium sulfide nanoparticles in zincblende phase and their magnetic properties.

    Science.gov (United States)

    Nakaya, Masafumi; Tanaka, Itaru; Muramatsu, Atsushi

    2012-12-01

    In this study, the random dope of Mn into CdS nanoparticles in zincblende phase has been carried out under the mild reaction condition. The resulting nanoparticles were characterized by energy dispersive X-ray analysis (EDX), transmission electron microscopy (TEM), X-ray diffractometer (XRD), UV-Vis spectrometer, PL spectrometer, and SQUID. EDX showed that the compositions of Mn doped CdS nanoparticles were readily controlled. TEM showed the particle sizes were not significantly affected by the compositions, retaining to be ca. 3 nm with a narrow size distribution. UV-Vis and PL spectra of the resulting nanoparticles showed the intra-Mn level may be affected by the quantum size effect. SQUID measurement showed that the resulting nanoparticles showed diamagnetism, paramagnetism and superparamagnetism dependent on Mn content.

  6. Dopamine/TiO{sub 2} hybrid thin films prepared by the liquid phase deposition method

    Energy Technology Data Exchange (ETDEWEB)

    Gutierrez-Tauste, David [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, Edifici Cn, 08290 Cerdanyola del Valles, Barcelona (Spain)], E-mail: davidg@qf.uab.es; Domenech, Xavier [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, Edifici Cn, 08290 Cerdanyola del Valles, Barcelona (Spain); Domingo, Concepcion [Instituto de Ciencia de Materiales (CSIC), Campus UAB, 08290 Cerdanyola del Valles, Barcelona (Spain); Ayllon, Jose A. [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, Edifici Cn, 08290 Cerdanyola del Valles, Barcelona (Spain)

    2008-04-30

    Liquid phase deposition method is applied to one-step production of a hybrid material composed by dopamine(DA) and TiO{sub 2} anatase. An optimized amount of the enediol derivative is added to a fluoride titania precursor aqueous solution in order to entrap this modifier within the growing TiO{sub 2}, yielding a DA/TiO{sub 2} nanocomposite material. Uniform, well-adhered and brown-colored thin films are deposited on indium tin oxide covered glass substrate. The DA/TiO{sub 2} hybrid material has been characterized by infrared spectroscopy, electronic microscopy, X-ray diffraction and UV-vis spectroscopy. The formation of the hybrid material seems to be reasonably explained by linkage of different TiO{sub 2} nanocrystallites taking advantage of both enediol and amine groups of DA.

  7. Extended phase homogeneity and electrical properties of barium calcium titanate prepared by the wet chemical methods

    International Nuclear Information System (INIS)

    Jayanthi, S.; Kutty, T.R.N.

    2004-01-01

    Ca-substituted BaTiO 3 with extended homogeneity range upto ∼50 mol% CaTiO 3 have been prepared by three different chemical routes namely carbonate-oxalate (COBCT), gel-carbonate (GCBCT), and gel-to-crystallite conversion (GHBCT) followed by heat treatment above 1150 deg. C. X-ray powder diffraction (XRD) data show continuous decrease in the tetragonal unit cell parameters as well as c 0 /a 0 ratio with CaTiO 3 content, which are in accordance with the substitution of smaller sized Ca 2+ ions at the barium sites. The microstructure as well as the dielectric properties are greatly influenced by the cationic ratio, α=(Ba+Ca)/Ti. The grain size decreases with CaTiO 3 content for the stoichiometric samples (α=1), whereas ultrafine microstructure is observed in the case of off-stoichiometric samples (α>1) for the whole compositional range of CaTiO 3 concentrations. Sharper ε r -T characteristics at lower calcium content and broader ε r -T with decreased ε max , in the higher calcium range are observed in the case of α=1. Whereas nanometer grained ceramics exhibiting diffuse ε r -T characteristics are obtained in the case of α>1. The positive temperature coefficient of resistivity (PTCR) is realized for barium calcium titanate ceramics having 0.3 at.% Sb as the donor dopant for higher CaTiO 3 (typically 30 mol%) containing samples (α=1), indicating that Ca 2+ ions do not behave as acceptors if they were to substitute at the Ti 4+ sites. Whereas the off-stoichiometric (α>1) ceramics retained high resistivity, indicative of the Ti-site occupancy for Ca 2+ in fine grain ceramics

  8. A review on procedures for the preparation of coatings for solid phase microextraction

    International Nuclear Information System (INIS)

    Aziz-Zanjani, Mohammad Ovais; Mehdinia, Ali

    2014-01-01

    Introduced in the 1990s, solid-phase microextraction (SPME) has found numerous applications. This is due to the solventless nature of SPME and the large variety of sorbents and coatings available. Highly diverse procedures have been applied to coat supports such as fused silica fibers or metal wires with sorbents in order to enhance capability, selectivity and robustness of SPME. Lately, research also is directed towards more simple methods for deposition of different types of coatings. Several of these methods have resulted in better stability and higher effective surface areas of the coatings. This review (with 128 references) covers the state of the art in methods for coating materials for use in SPME. It is divided into the following sections: (a) Dip methods and physical agglutination methods, (b) sol-gel technology, (c) chemical grafting, (d) electrochemical methods for coating (such as electrodeposition, anodizing and electrophoretic deposition), (e) electrospinning, (f) liquidphase deposition, and (g) hydrothermal methods. A final section covers conclusions and future trends. (author)

  9. Conformal and highly luminescent monolayers of Alq3 prepared by gas-phase molecular layer deposition.

    Science.gov (United States)

    Räupke, André; Albrecht, Fabian; Maibach, Julia; Behrendt, Andreas; Polywka, Andreas; Heiderhoff, Ralf; Helzel, Jonatan; Rabe, Torsten; Johannes, Hans-Hermann; Kowalsky, Wolfgang; Mankel, Eric; Mayer, Thomas; Görrn, Patrick; Riedl, Thomas

    2014-01-22

    The gas-phase molecular layer deposition (MLD) of conformal and highly luminescent monolayers of tris(8-hydroxyquinolinato)aluminum (Alq3) is reported. The controlled formation of Alq3 monolayers is achieved for the first time by functionalization of the substrate with amino groups, which serve as initial docking sites for trimethyl aluminum (TMA) molecules binding datively to the amine. Thereby, upon exposure to 8-hydroxyquinoline (8-HQ), the self-limiting formation of highly luminescent Alq3 monolayers is afforded. The growth process and monolayer formation were studied and verified by in situ quartz crystal monitoring, optical emission and absorption spectroscopy, and X-ray photoelectron spectroscopy. The nature of the MLD process provides an avenue to coat arbitrarily shaped 3D surfaces and porous structures with high surface areas, as demonstrated in this work for silica aerogels. The concept presented here paves the way to highly sensitive luminescent sensors and dye-sensitized metal oxides for future applications (e.g., in photocatalysis and solar cells).

  10. Effect of N-isopropylacrylamide on the preparation and properties of microencapsulated phase change materials

    International Nuclear Information System (INIS)

    Li, Dan; Wang, Jianping; Wang, Yanan; Li, Wei; Wang, Xuechen; Shi, Haifeng; Zhang, Xingxiang

    2016-01-01

    NIPAm (N-isopropylacrylamide), a thermosensitive monomer, was introduced into a system for synthesis of MicroPCMs (microencapsulated phase change materials) through free radical emulsion polymerization with n-oct (n-octadecane) as the core and cross-linked PMMA (poly (methyl methacrylate)) as the shell. The effect of NIPAm on the formation mechanism, surface morphologies, crystallization properties, and thermal stabilities of the MicroPCMs were studied using FTIR (Fourier transform infrared spectroscopy), SEM (scanning electron microscopy), DSC (differential scanning calorimetry), and TGA (thermogravimetric analysis), respectively. The results indicate that addition of NIPAm causes a significant increase in the enthalpy of the heterogeneous nucleation (approximately 2–4 times more than without NIPAm). The diameter distribution of microcapsules becomes narrower (the PDI (polydispersity index) has a minimum of 0.073) and the encapsulation ratio and encapsulation efficiency increase. On the contrary, the microcapsules that have some irregular holes were obtained by adding NIPAm prepolymer. - Highlights: • We designed and synthesized a lower supercooling microPCMs with the PNIPAm as nucleating agent. • Optimum dosage of monomer PNIPAm is 1.8 g. • The mass loss of microcapsules is less than 0.6% after repeated thermal cycling. • The formation mechanism of the microcapsules is discussed.

  11. Preparation of milk samples for immunoassay and liquid chromatographic screening using matrix solid-phase dispersion.

    Science.gov (United States)

    Barker, S A; Long, A R

    1994-01-01

    The use of drugs to maintain the health and maximize the output of dairy cattle has made the monitoring of milk for such agents essential. Screening tests based on immunological, microbial inhibition, and bacterial receptor assays have been developed for the detection of violative levels of therapeutic substances. However, such assays are not infallible, and false positive or negative results can occur when contaminants bind receptors or compete for the binding of the target residues. Such effects may arise from dietary sources, diseases, or other variables. Thus, a violation by such a test is not definitive until further confirmation is obtained. Our laboratory has developed extraction procedures for several drugs used in dairy production. Our method uses matrix solid-phase dispersion (MSPD) to isolate drugs away from contaminants and to eliminate many possible interferences. MSPD can also be used to enhance the specificity of such assays by fractionating various classes of drugs that may cross-react. Similarly, such methods may be used for liquid chromatographic screening and confirmation of a suspect sample.

  12. Chemical state and phase structure of (TaNbTiW)N films prepared by combined magnetron sputtering and PBII

    Energy Technology Data Exchange (ETDEWEB)

    Feng, Xingguo [State Key Laboratory of Advanced Welding and Joining, Harbin Institute of Technology, Harbin 150001 (China); Tang, Guangze [National Key Laboratory of Materials Behavior and Evaluation in Space Environment, Harbin Institute of Technology, Harbin 150001 (China); Sun, Mingren [National Key Laboratory of Science and Technology on Precision Hot Processing of Metals Harbin Institute of Technology, Harbin Institute of Technology, Harbin 150001 (China); Ma, Xinxin, E-mail: maxin@hit.edu.cn [State Key Laboratory of Advanced Welding and Joining, Harbin Institute of Technology, Harbin 150001 (China); Wang, Liqin [School of Mechatronics Engineering, Harbin Institute of Technology, Harbin, 150001 (China)

    2013-09-01

    (TaNbTiW)N films with thickness of ∼1000 nm are prepared on titanium alloy substrate by combined magnetron sputtering deposition and nitrogen plasma based ion implantation (N-PBII). Chemical state of the elements and phase structure of the films are investigated using X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD), respectively. The bonds of Ta-N, Nb-N, Ti-N-O and Ta-O are detected in the (TaNbTiW)N films, however both W-N and W-O are not found. The initial alloy film has a BCC structure, while the films with N-PBII treatment are composed of BCC and FCC structures. The hardness and elastic modulus of the films can be improved by increasing nitrogen implantation dose and reach maximum values of 9.0 GPa and 154.1 GPa, respectively.

  13. Preparation of a novel dual-function strong cation exchange/hydrophobic interaction chromatography stationary phase for protein separation.

    Science.gov (United States)

    Zhao, Kailou; Yang, Li; Wang, Xuejiao; Bai, Quan; Yang, Fan; Wang, Fei

    2012-08-30

    We have explored a novel dual-function stationary phase which combines both strong cation exchange (SCX) and hydrophobic interaction chromatography (HIC) characteristics. The novel dual-function stationary phase is based on porous and spherical silica gel functionalized with ligand containing sulfonic and benzyl groups capable of electrostatic and hydrophobic interaction functionalities, which displays HIC character in a high salt concentration, and IEC character in a low salt concentration in mobile phase employed. As a result, it can be employed to separate proteins with SCX and HIC modes, respectively. The resolution and selectivity of the dual-function stationary phase were evaluated under both HIC and SCX modes with standard proteins and can be comparable to that of conventional IEC and HIC columns. More than 96% of mass and bioactivity recoveries of proteins can be achieved in both HIC and SCX modes, respectively. The results indicated that the novel dual-function column could replace two individual SCX and HIC columns for protein separation. Mixed retention mechanism of proteins on this dual-function column based on stoichiometric displacement theory (SDT) in LC was investigated to find the optimal balance of the magnitude of electrostatic and hydrophobic interactions between protein and the ligand on the silica surface in order to obtain high resolution and selectivity for protein separation. In addition, the effects of the hydrophobicity of the ligand of the dual-function packings and pH of the mobile phase used on protein separation were also investigated in detail. The results show that the ligand with suitable hydrophobicity to match the electrostatic interaction is very important to prepare the dual-function stationary phase, and a better resolution and selectivity can be obtained at pH 6.5 in SCX mode. Therefore, the dual-function column can replace two individual SCX and HIC columns for protein separation and be used to set up two-dimensional liquid

  14. Effect Anticipation Affects Perceptual, Cognitive, and Motor Phases of Response Preparation: Evidence from an Event-Related Potential (ERP) Study

    Science.gov (United States)

    Harrison, Neil R.; Ziessler, Michael

    2016-01-01

    The anticipation of action effects is a basic process that can be observed even for key-pressing responses in a stimulus-response paradigm. In Ziessler et al.’s (2012) experiments participants first learned arbitrary effects of key-pressing responses. In the test phase an imperative stimulus determined the response, but participants withheld the response until a Go-stimulus appeared. Reaction times (RTs) were shorter if the Go-stimulus was compatible with the learned response effect. This is strong evidence that effect representations were activated during response planning. Here, we repeated the experiment using event-related potentials (ERPs), and we found that Go-stimulus locked ERPs depended on the compatibility relationship between the Go-stimulus and the response effect. In general, this supports the interpretation of the behavioral data. More specifically, differences in the ERPs between compatible and incompatible Go-stimuli were found for the early perceptual P1 component and the later frontal P2 component. P1 differences were found only in the second half of the experiment and for long stimulus onset asynchronies (SOAs) between imperative stimulus and Go-stimulus, i.e., when the effect was fully anticipated and the perceptual system was prepared for the effect-compatible Go-stimulus. P2 amplitudes, likely associated with evaluation and conflict detection, were larger when Go-stimulus and effect were incompatible; presumably, incompatibility increased the difficulty of effect anticipation. Onset of response-locked lateralized readiness potentials (R-LRPs) occurred earlier under incompatible conditions indicating extended motor processing. Together, these results strongly suggest that effect anticipation affects all (i.e., perceptual, cognitive, and motor) phases of response preparation. PMID:26858621

  15. Effect anticipation affects perceptual, cognitive, and motor phases of response preparation: evidence from an event-related potential (ERP study

    Directory of Open Access Journals (Sweden)

    Neil Richard Harrison

    2016-01-01

    Full Text Available The anticipation of action effects is a basic process that can be observed even for key-pressing responses in a stimulus-response paradigm. In Ziessler, Nattkemper and Vogt’s (2012 experiments participants first learned arbitrary effects of key-pressing responses. In the test phase an imperative stimulus determined the response, but participants withheld the response until a Go-stimulus appeared. Reaction times were shorter if the Go-stimulus was compatible with the learned response effect. This is strong evidence that effect representations were activated during response planning. Here we repeated the experiment using event-related potentials (ERPs, and we found that Go-stimulus locked ERPs depended on the compatibility relationship between the Go-stimulus and the response effect. In general, this supports the interpretation of the behavioural data. More specifically, differences in the ERPs between compatible and incompatible Go-stimuli were found for the early perceptual P1 component and the later frontal P2 component. P1 differences were found only in the second half of the experiment and for long SOAs between imperative stimulus and Go-stimulus, i.e. when the effect was fully anticipated and the perceptual system was prepared for the effect-compatible Go-stimulus. P2 amplitudes, likely associated with evaluation and conflict detection, were larger when Go-stimulus and effect were incompatible; presumably, incompatibility increased the difficulty of effect anticipation. Onset of response-locked LRPs occurred earlier under incompatible conditions indicating extended motor processing. Together, these results strongly suggest that effect anticipation affects all (i.e. perceptual, cognitive, and motor phases of response preparation.

  16. Effect Anticipation Affects Perceptual, Cognitive, and Motor Phases of Response Preparation: Evidence from an Event-Related Potential (ERP) Study.

    Science.gov (United States)

    Harrison, Neil R; Ziessler, Michael

    2016-01-01

    The anticipation of action effects is a basic process that can be observed even for key-pressing responses in a stimulus-response paradigm. In Ziessler et al.'s (2012) experiments participants first learned arbitrary effects of key-pressing responses. In the test phase an imperative stimulus determined the response, but participants withheld the response until a Go-stimulus appeared. Reaction times (RTs) were shorter if the Go-stimulus was compatible with the learned response effect. This is strong evidence that effect representations were activated during response planning. Here, we repeated the experiment using event-related potentials (ERPs), and we found that Go-stimulus locked ERPs depended on the compatibility relationship between the Go-stimulus and the response effect. In general, this supports the interpretation of the behavioral data. More specifically, differences in the ERPs between compatible and incompatible Go-stimuli were found for the early perceptual P1 component and the later frontal P2 component. P1 differences were found only in the second half of the experiment and for long stimulus onset asynchronies (SOAs) between imperative stimulus and Go-stimulus, i.e., when the effect was fully anticipated and the perceptual system was prepared for the effect-compatible Go-stimulus. P2 amplitudes, likely associated with evaluation and conflict detection, were larger when Go-stimulus and effect were incompatible; presumably, incompatibility increased the difficulty of effect anticipation. Onset of response-locked lateralized readiness potentials (R-LRPs) occurred earlier under incompatible conditions indicating extended motor processing. Together, these results strongly suggest that effect anticipation affects all (i.e., perceptual, cognitive, and motor) phases of response preparation.

  17. Effect of kaolin particle size and loading on the characteristics of kaolin ceramic support prepared via phase inversion technique

    Directory of Open Access Journals (Sweden)

    Siti Khadijah Hubadillah

    2016-06-01

    Full Text Available In this study, low cost ceramic supports were prepared from kaolin via phase inversion technique with two kaolin particle sizes, which are 0.04–0.6 μm (denoted as type A and 10–15 μm (denoted as type B, at different kaolin contents ranging from 14 to 39 wt.%, sintered at 1200 °C. The effect of kaolin particle sizes as well as kaolin contents on membrane structure, pore size distribution, porosity, mechanical strength, surface roughness and gas permeation of the support were investigated. The support was prepared using kaolin type A induced asymmetric structure by combining macroporous voids and sponge-like structure in the support with pore size of 0.38 μm and 1.05 μm, respectively, and exhibited ideal porosity (27.7%, great mechanical strength (98.9 MPa and excellent gas permeation. Preliminary study shows that the kaolin ceramic support in this work is potential to gas separation application at lower cost.

  18. Characteristic of New Solid-Phase Extraction Sorbent: Activated Carbon Prepared from Rice Husks under Base Treated Condition

    Directory of Open Access Journals (Sweden)

    Afrida Kurnia Putri

    2012-10-01

    Full Text Available A characterization of activated carbon (ACs prepared from rice husks (RHs under base treated condition as a new sorbent for solid-phase extraction (SPE to extract 4-nonylphenol isomers (4-NPs in water samples has been done. The ACs prepared from RHs usually exhibits low specific surface area due to its high ash content, but in case of its application for SPE, there are other factors need to be considered, such as the existence of functional groups inside the sorbent, that can enhance interaction of non-polar sorbent with analyte in the water matrices. In this case, silanol groups from ash content may affect the extraction efficiency for 4-NPs. The ACs made from RHs were chemically impregnated with ZnCl2 and carbonized at 800oC. To investigate the role of silica, three types of ACs were prepared, i.e., untreated ACs (AC–Si, contain silica, base treated ACs (AC–B–Si, remain some silica inside, and ACs made by base treated RHs (AC–B, no silica, the surface area obtained from these treatments were 1352 m2/g, 1666 m2/g, and 1712m2/g respectively.  ACs made by base treatment has the highest surface area (related to BET, which indicat that silica removal process promotes the formation of open pore system on ACs and enhances the surface area of ACs. However, extraction efficiency measured by GC-MS in SPE process showed the reversal trends (i.e., AC–Si= 32.08%, AC–B–Si= 82.63%, AC–B=51.78%, among them the AC–B–Si sorbent reveal the best performance in SPE process. It is indicated that although silica usually exhibits low specific surface area, but control presence of silica as a polar functional group has a positive influence in the interaction between non-polar sorbent and 4-NPs.

  19. Polypyrrole solid phase microextraction: A new approach to rapid sample preparation for the monitoring of antibiotic drugs

    International Nuclear Information System (INIS)

    Szultka, Malgorzata; Kegler, Ricarda; Fuchs, Patricia; Olszowy, Pawel; Miekisch, Wolfram; Schubert, Jochen K.; Buszewski, Boguslaw; Mundkowski, Ralf G.

    2010-01-01

    Simple or even rapid bioanalytical methods are rare, since they generally involve complicated, time-consuming sample preparation from the biological matrices like LLE or SPE. SPME provides a promising approach to overcome these limitations. The full potential of this innovative technique for medical diagnostics, pharmacotherapy or biochemistry has not been tapped yet. In-house manufactured SPME probes with polypyrrole (PPy) coating were evaluated using three antibiotics of high clinical relevance - linezolid, daptomycin, and moxifloxacin - from PBS, plasma, and whole blood. The PPy coating was characterised by scanning electron microscopy. Influences of pH, inorganic salt, and blood anticoagulants were studied for optimum performance. Extraction yields were determined from stagnant media as well as re-circulating human blood using the heart-and-lung machine model system. The PPy-SPME fibres showed high extraction yields, particularly regarding linezolid. The reproducibility of the method was optimised to achieve RSDs of 9% or 17% and 7% for SPME from stagnant or re-circulating blood using fresh and re-used fibres, respectively. The PPy-SPME approach was demonstrated to meet the requirements of therapeutic monitoring of the drugs tested, even from re-circulating blood at physiological flow rates. SPME represents a rapid and simple dual-step procedure with potency to significantly reduce the effort and expenditure of complicated sample preparations in biomedical analysis.

  20. Polypyrrole solid phase microextraction: A new approach to rapid sample preparation for the monitoring of antibiotic drugs

    Energy Technology Data Exchange (ETDEWEB)

    Szultka, Malgorzata [Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus, Copernicus University, Gagarin 7, 87-100 Torun (Poland); Kegler, Ricarda [Institute of Clinical Pharmacology, University of Rostock, Schillingallee 70, D-18057 Rostock (Germany); Fuchs, Patricia [Department of Anaesthesia and Intensive Care, University of Rostock, Schillingallee 35, D-18057 Rostock (Germany); Olszowy, Pawel [Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus, Copernicus University, Gagarin 7, 87-100 Torun (Poland); Miekisch, Wolfram; Schubert, Jochen K. [Department of Anaesthesia and Intensive Care, University of Rostock, Schillingallee 35, D-18057 Rostock (Germany); Buszewski, Boguslaw [Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus, Copernicus University, Gagarin 7, 87-100 Torun (Poland); Mundkowski, Ralf G., E-mail: ralf.mundkowski@med.uni-rostock.de [Institute of Clinical Pharmacology, University of Rostock, Schillingallee 70, D-18057 Rostock (Germany)

    2010-05-14

    Simple or even rapid bioanalytical methods are rare, since they generally involve complicated, time-consuming sample preparation from the biological matrices like LLE or SPE. SPME provides a promising approach to overcome these limitations. The full potential of this innovative technique for medical diagnostics, pharmacotherapy or biochemistry has not been tapped yet. In-house manufactured SPME probes with polypyrrole (PPy) coating were evaluated using three antibiotics of high clinical relevance - linezolid, daptomycin, and moxifloxacin - from PBS, plasma, and whole blood. The PPy coating was characterised by scanning electron microscopy. Influences of pH, inorganic salt, and blood anticoagulants were studied for optimum performance. Extraction yields were determined from stagnant media as well as re-circulating human blood using the heart-and-lung machine model system. The PPy-SPME fibres showed high extraction yields, particularly regarding linezolid. The reproducibility of the method was optimised to achieve RSDs of 9% or 17% and 7% for SPME from stagnant or re-circulating blood using fresh and re-used fibres, respectively. The PPy-SPME approach was demonstrated to meet the requirements of therapeutic monitoring of the drugs tested, even from re-circulating blood at physiological flow rates. SPME represents a rapid and simple dual-step procedure with potency to significantly reduce the effort and expenditure of complicated sample preparations in biomedical analysis.

  1. Preparation and evaluation of a hydrophilic interaction and cation-exchange chromatography stationary phase modified with 2-methacryloyloxyethyl phosphorylcholine.

    Science.gov (United States)

    Xiong, Caifeng; Yuan, Jie; Wang, Zhiying; Wang, Siyao; Yuan, Chenchen; Wang, Lili

    2018-04-20

    In this work, 2-methacryloyloxyethyl phosphorylcholine (MPC) was used as a ligand to prepare a novel mixed-mode chromatography (MMC) stationary phase by the thiol-ene click reaction onto silica (MPC-silica). It was found that this MPC-silica showed the retention characteristics of hydrophilic interaction chromatography (HILIC) and weak cation exchange chromatography (WCX) under suitable mobile phase conditions. In detail, acidic and basic hydrophilic compounds and puerarin from pueraria were separated quickly with HILIC mode. Meanwhile, six standard proteins were allowed to reach baseline separation in WCX mode, and protein separation from egg white was also achieved with this mode. In addition, reduced/denatured lysozyme could be refolded with the MPC-silica column. In the meantime, the MPC-silica has been applied for refolding with simultaneous purification of recombinant human Delta-like1-RGD (rhDll1-RGD) expressed in Escherichia coli. The results show that the mass recovery and purity of rhDll1-RGD could reach 63.4% and 97% by one step, respectively. Furthermore, the reporter assay results demonstrated that refolded with simultaneously purified rhDll1-RGD could efficiently activate the signalling pathway in a dose-dependent manner. In general, this MPC-silica has good resolution and selectivity in the separation of polar compounds and protein samples in different high-performance liquid chromatography (HPLC) modes, and it successfully achieved refolding with simultaneous purification of denatured protein. Copyright © 2018 Elsevier B.V. All rights reserved.

  2. A new polyethylene glycol fiber prepared by coating porous zinc electrodeposited onto silver for solid-phase microextraction of styrene

    International Nuclear Information System (INIS)

    Sungkaew, Sakchaibordee; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

    2010-01-01

    A new polyethylene glycol fiber was developed for solid-phase microextraction (SPME) of styrene by electrodepositing porous Zn film on Ag wire substrate followed by coating with polyethylene glycol sol-gel (Ag/Zn/PEG sol-gel fiber). The scanning electron micrographs of fibers surface revealed a highly porous structure. The extraction property of the developed fiber-to-styrene residue from polystyrene packaged food was investigated by headspace solid-phase microextraction (HS-SPME) and analyzed with a gas chromatograph coupled with flame ionization detection (GC-FID). The new Ag/Zn/PEG sol-gel fiber is simple to prepare, low cost, robust, has high thermal stability and long lifetime, up to 359 extractions. Repeatability of one fiber (n = 6) was in the range of 4.7-7.5% and fiber-to-fiber reproducibility (n = 4) for five concentration values were in the range 3.4-10%. This Ag/Zn/PEG sol-gel fiber was compared to two commercial SPME fibers, 75 μm carboxen/polydimethylsiloxane (CAR/PDMS) and 100 μm polydimethylsiloxane (PDMS). Under their optimum conditions, Ag/Zn/PEG sol-gel fiber showed the highest sensitivity and the lowest detection limit at 0.28 ± 0.01 ng mL -1 .

  3. Butanol Dehydration over V₂O₅-TiO₂/MCM-41 Catalysts Prepared via Liquid Phase Atomic Layer Deposition.

    Science.gov (United States)

    Choi, Hyeonhee; Bae, Jung-Hyun; Kim, Do Heui; Park, Young-Kwon; Jeon, Jong-Ki

    2013-04-29

    MCM-41 was used as a support and, by using atomic layer deposition (ALD) in the liquid phase, a catalyst was prepared by consecutively loading titanium oxide and vanadium oxide to the support. This research analyzes the effect of the loading amount of vanadium oxide on the acidic characteristics and catalytic performance in the dehydration of butanol. The physical and chemical characteristics of the TiO₂-V₂O₅/MCM-41 catalysts were analyzed using XRF, BET, NH₃-TPD, XRD, Py-IR, and XPS. The dehydration reaction of butanol was performed in a fixed bed reactor. For the samples with vanadium oxide loaded to TiO₂/MCM-41 sample using the liquid phase ALD method, it was possible to increase the loading amount until the amount of vanadium oxide reached 12.1 wt %. It was confirmed that the structural properties of the mesoporous silica were retained well after titanium oxide and vanadium loading. The NH₃-TPD and Py-IR results indicated that weak acid sites were produced over the TiO₂/MCM-41 samples, which is attributed to the generation of Lewis acid sites. The highest activity of the V₂O₅(12.1)-TiO₂/MCM-41 catalyst in 2-butanol dehydration is ascribed to it having the highest number of Lewis acid sites, as well as the highest vanadium dispersion.

  4. Preparation and characterization of Ge2Sb2Te5 phase change films on elastic substrates by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Hongbing; Thelander, Erik; Benke, Julia; Rauschenbach, Bernd [Leibniz Institute of Surface Modification, 04318 Leipzig (Germany)

    2012-07-01

    Ge{sub 2}Sb{sub 2}Te{sub 5} (GST) thin films have attracted a great deal of interest as an active layer for data storage media due to its high switching rate and extremely good reversibility. Here we demonstrate the preparation of high-quality GST films on elastic polyimide substrates by pulsed laser deposition (PLD). The composition and chemical state of the films were investigated by energy dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS), respectively. The effect of annealing temperature on the crystalline nature of the films was also studied. As-deposited films were found to be amorphous. Crystalline phases with face-centered cubic and hexagonal structures appeared at 180 and 300 degrees, respectively. Importantly, no phase separation could be seen in the annealed films. Furthermore, reflectivity measurements were performed to characterize the as-deposited and annealed films, showing a high reflectivity contrast (up to 23%) between full crystalline and amorphous films. Our results indicate that PLD deposited GST film on polyimide substrate is a promising candidate for use in future flexible memory devices.

  5. A bioinspired polydopamine approach toward the preparation of gold-modified magnetic nanoparticles for the magnetic solid-phase extraction of steroids in multiple samples.

    Science.gov (United States)

    An, Xuehan; Chai, Weibo; Deng, Xiaojuan; Chen, Hui; Ding, Guosheng

    2018-05-02

    In this work, a simple, facile, and sensitive magnetic solid-phase extraction method was developed for the extraction and enrichment of three representative steroid hormones before high-performance liquid chromatography analysis. Gold-modified Fe 3 O 4 nanoparticles, as novel magnetic adsorbents, were prepared by a rapid and environmentally friendly procedure in which polydopamine served as the reductant as well as the stabilizer for the gold nanoparticles, thus successfully avoiding the use of some toxic reagents. To obtain maximum extraction efficiency, several significant factors affecting the preconcentration steps, including the amount of adsorbent, extraction time, pH of the sample solution, and the desorption conditions, were optimized, and the enrichment factors for three steroids were all higher than 90. The validity of the established method was evaluated and good analytical characteristics were obtained. A wide linearity range (0.8-500 μg/L for all the analytes) was attained with good correlation (R 2  ≥ 0.991). The low limits of detection were 0.20-0.25 μg/L, and the relative standard deviations ranged from 0.83 to 4.63%, demonstrating a good precision. The proposed method was also successfully applied to the extraction and analysis of steroids in urine, milk, and water samples with satisfactory results, which showed its reliability and feasibility in real sample analysis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Preparation, morphology and thermal properties of electrospun fatty acid eutectics/polyethylene terephthalate form-stable phase change ultrafine composite fibers for thermal energy storage

    International Nuclear Information System (INIS)

    Cai Yibing; Ke Huizhen; Lin Liang; Fei Xiuzhu; Wei Qufu; Song Lei; Hu Yuan; Fong Hao

    2012-01-01

    Highlights: ► Electrospun binary fatty acid eutectics/PET ultrafine composite fibers were prepared. ► Fatty acid eutectics had appropriate phase transition temperature and heat enthalpy. ► Their morphological structures and thermal properties were different from each other. ► Composite fibers could be innovative form-stable PCMs for thermal energy storage. - Abstract: The ultrafine composite fibers based on the composites of binary fatty acid eutectics and polyethylene terephthalate (PET) with varied fatty acid eutectics/PET mass ratios (50/100, 70/100, 100/100 and 120/100) were fabricated using the technique of electrospinning as form-stable phase change materials (PCMs). The five binary fatty acid eutectics including LA–MA, LA–PA, MA–PA, MA–SA and PA–SA were prepared according to Schrader equation, and then were selected as an innovative type of solid–liquid PCMs. The results characterized by differential scanning calorimeter (DSC) indicated that the prepared binary fatty acid eutectics with low phase transition temperatures and high heat enthalpies for climatic requirements were more suitable for applications in building energy storage. The structural morphologies, thermal energy storage and thermal stability properties of the ultrafine composite fibers were investigated by scanning electron microscope (SEM), DSC and thermogravimetric analysis (TGA), respectively. SEM images revealed that the electrospun binary fatty acid eutectics/PET ultrafine composite fibers possessed the wrinkled surfaces morphologies compared with the neat PET fibers with cylindrical shape and smooth surfaces; the grooves or ridges on the corrugated surface of the ultrafine composite fibers became more and more prominent with increasing fatty acid eutectics amount in the composite fibers. The fibers with the low mass ratio maintained good structural morphologies while the quality became worse when the mass ratio is too high (more than 100/100). DSC measurements

  7. Janus graphene oxide nanosheet: A promising additive for enhancement of polymeric membranes performance prepared via phase inversion.

    Science.gov (United States)

    Akbari, Mahdi; Shariaty-Niassar, Mojtaba; Matsuura, Takeshi; Ismail, Ahmad Fauzi

    2018-10-01

    Although polymeric membranes find important role in water and waste water treatment in recent years, their fouling is still an important problem. Application of hydrophilic nanoparticles (NPs) is one of the proposed methods for reducing fouling of membranes but their dispersion and stability in hydrophobic polymer matrix is challenging. In this study Janus functionalization of the NPs was introduced as a promising technique toward achieving this goal. Polysulfone (PSf) membranes containing various concentrations of graphene oxide (GO) nanosheets and Janus graphene oxide (Janus GO) nanosheets (as additives) were fabricated via phase inversion. The synthesized nanosheets were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy and dynamic light scattering (DLS). The prepared membranes also were then characterized by scanning electron microscopy (SEM), contact angle (CA), water uptake, porosity, mean pore size and casting solution viscosity. The membrane performance was also tested by determining pure water flux (PWF), bovine serum albumin (BSA) separation, flux reduction by fouling and flux recovery. CA reduced from 85° to 68° and PWF increased from 23.15 L/m 2  h to 230.61 L/m 2  h for PSF and Janus GO nanosheets containing membrane, respectively. Also investigation of antifouling performance of membranes revealed that membrane with the 1 wt.% of Janus GO nanosheets had higher water flux recovery ratio (FRR) and lower irreversible fouling (R ir ) of 84% and 16%, respectively. These improvements were attributed to the better dispersion and stability of Janus GO nanosheets in the prepared mixed matrix membranes. Copyright © 2018 Elsevier Inc. All rights reserved.

  8. Preparation and properties of poly(vinyl alcohol)-g-octadecanol copolymers based solid–solid phase change materials

    International Nuclear Information System (INIS)

    Shi Haifeng; Li Jianhua; Jin Yanmei; Yin Yiping; Zhang Xingxiang

    2011-01-01

    Highlights: ► In this paper, our objective is just focused on the preparation and characterization of such SSPCMs aiming at providing one suitable material for improving the thermal stability and preventing the liquid leakage from the matrix. Here, the SSPCMs can be fabricated by grafting to method between poly(vinyl alcohol) and octadecanol, which the grafting ratio can be controlled by adjusting the feeding components. ► The thermal properties, crystalline structure and morphology were detailed studies by WAXD, FT-IR, TGA and DSC, proving that the PVA-g-octadecanol process the better thermal storage ability and thermal stability. Compared with pure octadecanol, the heat fusion of PVA-g-octadecanol decreased due to the mobility confinement and the lower rearrangements of C18 alkyl side chains. ► This result is for the first time reported, and is a meaningful result for the investigation of the solid–solid phase change materials, and the preparation process provides one template-directed approach to obtain the high-performance materials with the better heat storage and thermal stability. - Abstract: The heat storage and phase transition behavior of a series of poly(vinyl alcohol)-g-octadecanol copolymers (PVA-g-C18OH) with apparent grafting ratios ranging from 283 to 503%, synthesized through “grafting to” method, has been investigated by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), wide-angle X-ray diffraction (WAXD) and polarized optical microscopy (POM). PVA-g-C18OH copolymers exhibit the better thermal stability against C18OH, and the thermal energy storage ability (ΔH m ) is of dependence on the apparent grafting ratios. Compared with C18OH, the lower thermal storage efficiency possible is attributed to the less CH 2 groups entered into the crystalline domains and the frustrated mobility of the grafted C18 alkyl side chains between PVA backbones. The results show that

  9. Preparation and thermal performance of polystyrene/n-tetradecane composite nanoencapsulated cold energy storage phase change materials

    International Nuclear Information System (INIS)

    Fang, Yutang; Yu, Huimin; Wan, Weijun; Gao, Xuenong; Zhang, Zhengguo

    2013-01-01

    Highlights: • Average particle size of Tet/PS nanocapsules is smaller than the same type composite. • Latent heat of Tet/PS nanocapsules is as high as the same type composite. • Freeze–thaw cycle test and centrifugal sedimentation method are employed. • Tet/PS nanocapsules can be a candidate for cold thermal energy storage. - Abstract: In this paper, a novel polystyrene/n-tetradecane composite nanoencapsulated phase change material as latent functionally thermal fluid (LFTF) for cold thermal energy storage was synthesized by ultrasonic-assistant miniemulsion in situ polymerization. The morphology, chemical structure and thermal performances of the nanoencapsulated phase change material (NEPCM) were measured by particle size analyzer, transmission electron microscope (TEM), Fourier transform infrared (FT-IR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TG), respectively. The thermo-physical properties of the cool storage media were tested as well. The results showed that, a uniform spherical NEPCM with average diameter of 132 nm was prepared. The melting and freezing points and the latent heats of the NEPCMs was measured as 4.04 °C and −3.43 °C, 98.71 J g −1 and 91.27 J g −1 , respectively. The specific heat of its latex were determined as the maximum value of 4.822 J g −1 K −1 . The freeze–thaw cycle test indicated that the NEPCMs have good mechanical stability, and most capsules were still complete except some broken individuals from TEM images. Due to its good thermal properties and mechanical stability, the polystyrene/n-tetradecane NEPCM displays a good potential for cool energy storage

  10. Preparation and flammability of high density polyethylene/paraffin/organophilic montmorillonite hybrids as a form stable phase change material

    International Nuclear Information System (INIS)

    Cai, Yibing; Hu, Yuan; Song, Lei; Kong, Qinghong; Yang, Rui; Zhang, Yinping; Chen, Zuyao; Fan, Weicheng

    2007-01-01

    A kind of form stable phase change material (PCM) based on high density polyethylene (HDPE), paraffin, organophilic montmorillonite (OMT) and intumescent flame retardant (IFR) hybrids is prepared by using a twin screw extruder technique. This kind of form stable PCM is made of paraffin as a dispersed phase change material and HDPE as a supporting material. The structure of the montmorillonite (MMT) and OMT is characterized by X-ray diffraction (XRD) and high resolution electron microscopy (HREM). The analysis indicates that the MMT is a kind of lamellar structure, and the structure does not change after organic modification. However, the structure of the hybrid is evidenced by the XRD and scanning electronic microscope (SEM). Its thermal stability, latent heat and flame retardant properties are given by the Thermogravimetry analysis (TGA), differential scanning calorimeter (DSC) method and cone calorimeter, respectively. Synergy is observed between the OMT and IFR. The XRD result indicates that the paraffin intercalates into the silicate layers of the OMT, thus forming a typically intercalated hybrid. The SEM investigation and DSC result show that the additives of OMT and IFR have hardly any effect on the HDPE/paraffin three dimensional netted structure and the latent heat. In TGA curves, although the onset of weight loss of flame-retardant form stable PCMs occur at a lower temperature than that of form stable PCM, flame-retardant form stable PCMs produce a large amount of char residue at 700 o C. The synergy between OMT and IFR leads to the decrease of the heat release rate (HRR), contributing to improvement of the flammability performance

  11. Strong and biocompatible three-dimensional porous silk fibroin/graphene oxide scaffold prepared by phase separation.

    Science.gov (United States)

    Wang, Shu-Dong; Ma, Qian; Wang, Ke; Ma, Pi-Bo

    2018-05-01

    Silk fibroin (SF) is blended with graphene oxide (GO) to prepare the strong and biocompatible three dimensional porous SF/GO blended scaffold via phase separation. GO could be well dispersed in SF solution and GO could also be well distributed in the SF scaffold. Furthermore, the introduction of GO can lead to structural change in the bended scaffold. Higher concentration of GO resulted in more compact structure and smaller pore size of the composite scaffolds without decreasing their porosity. Scanning electron microscopy and energy dispersive spectrometry results also reveal that SF and GO are homogeneous blended together. Analysis of chemical structures of the scaffold shows that addition of GO do not affect the crystalline structure of SF and it is evenly blended with SF. The blended scaffold has significantly higher breaking strength than the pure SF scaffold. In vitro study indicates that both pure SF scaffold and SF/GO composite scaffold support growth and proliferation of MC3T3-E1 osteoprogenitor cells. However, the addition of GO contribute to the proliferation of MC3T3-E1 osteoprogenitor. The testing results show that the blended scaffold is an appropriate candidate for tissue engineering. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

    2013-07-01

    A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Graphene nanosheets preparation using magnetic nanoparticle assisted liquid phase exfoliation of graphite: The coupled effect of ultrasound and wedging nanoparticles.

    Science.gov (United States)

    Hadi, Alireza; Zahirifar, Jafar; Karimi-Sabet, Javad; Dastbaz, Abolfazl

    2018-06-01

    This study aims to investigate a novel technique to improve the yield of liquid phase exfoliation of graphite to graphene sheets. The method is based on the utilization of magnetic Fe 3 O 4 nanoparticles as "particle wedge" to facilitate delamination of graphitic layers. Strong shear forces resulted from the collision of Fe 3 O 4 particles with graphite particles, and intense ultrasonic waves lead to enhanced exfoliation of graphite. High quality of graphene sheets along with the ease of Fe 3 O 4 particle separation from graphene solution which arises from the magnetic nature of Fe 3 O 4 nanoparticles are the unique features of this approach. Initial graphite flakes and produced graphene sheets were characterized by various methods including field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Raman spectroscopy, atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and Zeta potential analysis. Moreover, the effect of process factors comprising initial graphite concentration, Fe 3 O 4 nanoparticles concentration, sonication time, and sonication power were investigated. Results revealed that graphene preparation yield and the number of layers could be manipulated by the presence of magnetic nanoparticles. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. Preparation of microporous Cellulose/Poly(vinylidene fluoride-hexafluoropropylene) membrane for lithium ion batteries by phase inversion method

    Science.gov (United States)

    Asghar, Muhammad Rehman; Zhang, Yao; Wu, Aiming; Yan, Xiaohui; Shen, Shuiyun; Ke, Changchun; Zhang, Junliang

    2018-03-01

    In this work, a porous and honeycomb-structured Cellulose/Poly (vinylidene fluoride-hexafluoropropylene) (PVDF-HFP) membrane is prepared via a facile and ecofriendly phase inversion method by using glycerol as pore forming agent. Cellulose acetate, the source of cellulose, is easily converted into cellulose by hydrolysis in the presence of lithium hydroxide. Owing to the unique microstructure, the Cellulose/PVDF-HFP membrane offers several advantages, including high porosity, elevated electrolyte uptake, high ion conductivity, and wide electrochemical window (5.35 V). Compared with conventional polypropylene (PP) separator and PVDF-HFP membrane, the membrane developed in this work enables higher discharge capacity, higher lithium-ion transference number (0.89) and improved rate performance, which is able to maintain a high discharge capacity of 136 mAh g-1 at 8 C, using LiCoO2 as cathode and Li metal as anode. In addition, the Cellulose/PVDF-HFP membrane based batteries exhibit superior cycling performance that can maintain 91.7% capacity after 100 cycles at 0.2 C. The characterization and battery test results demonstrate that the membrane is highly compatible with lithium ion batteries.

  15. Combining Pickering Emulsion Polymerization with Molecular Imprinting to Prepare Polymer Microspheres for Selective Solid-Phase Extraction of Malachite Green

    Directory of Open Access Journals (Sweden)

    Weixin Liang

    2017-08-01

    Full Text Available Malachite green (MG is currently posing a carcinogenic threat to the safety of human lives; therefore, it is highly desirable to develop an effective method for fast trace detection of MG. Herein, for the first time, this paper presents a systematic study on polymer microspheres, being prepared by combined Pickering emulsion polymerization and molecular imprinting, to detect and purify MG. The microspheres, molecularly imprinted with MG, show enhanced adsorption selectivity to MG, despite a somewhat lowered adsorption capacity, as compared to the counterpart without molecular imprinting. Structural features and adsorption performance of these microspheres are elucidated by different characterizations and kinetic and thermodynamic analyses. The surface of the molecularly imprinted polymer microspheres (M-PMs exhibits regular pores of uniform pore size distribution, endowing M-PMs with impressive adsorption selectivity to MG. In contrast, the microspheres without molecular imprinting show a larger average particle diameter and an uneven porous surface (with roughness and a large pore size, causing a lower adsorption selectivity to MG despite a higher adsorption capacity. Various adsorption conditions are investigated, such as pH and initial concentration of the solution with MG, for optimizing the adsorption performance of M-PMs in selectively tackling MG. The adsorption kinetics and thermodynamics are deeply discussed and analyzed, so as to provide a full picture of the adsorption behaviors of the polymer microspheres with and without the molecular imprinting. Significantly, M-PMs show promising solid-phase extraction column applications for recovering MG in a continuous extraction manner.

  16. Reactivity of main components and substituent distribution in esterified sugarcane bagasse prepared by effective solid phase reaction.

    Science.gov (United States)

    Gan, Tao; Zhang, Yanjuan; Chen, Yane; Hu, Huayu; Yang, Mei; Huang, Zuqiang; Chen, Dong; Huang, Aimin

    2018-02-01

    Three main components of lignocellulose (cellulose, hemicellulose, and lignin isolated from sugarcane bagasse (SCB)) as well as holocellulose and SCB were modified with maleic acid by mechanical activation (MA)-assisted solid phase reaction (MASPR) technology. The order of reactivity was found to be lignin>hemicellulose>cellulose. The amorphous structure of lignin and hemicellulose mainly attributed to their better reactivity, and the modified lignin could reach a maximum degree of esterification (DE) of 93.45%. MA improved the accessibility and reactivity of cellulose, as the DE of modified cellulose gradually increased with milling time and reached the maximum value of 57.30% at 120min, which had significant effect on structure changes and DE of modified holocellulose and SCB. MA enhanced the esterification of all three components in lignocellulose with relatively high substituent distribution in them, and maleated SCB with a maximum DE of 64.17% was successfully prepared by this simple, green, and effective MASPR technology. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Preparation and thermo-optical characteristics of a smart polymer-stabilized liquid crystal thin film based on smectic A–chiral nematic phase transition

    International Nuclear Information System (INIS)

    Sun, Jian; Wang, Huihui; Cao, Hui; Ding, Hangjun; Yang, Zhou; Yang, Huai; Wang, Ling; Xie, Hui; Luo, Xueyao; Xiao, Jiumei

    2014-01-01

    A smart polymer stabilized liquid crystal (PSLC) thin film with temperature-controllable light transmittance was prepared based on a smectic-A (SmA)–chiral nematic (N*) phase transition, and then the effect of the composition and the preparation condition of the PSLC film on its thermo-optical (T-O) characteristics has been investigated in detail. Within the temperature range of the SmA phase, the PSLC shows a strong opaque state due to the focal conic alignment of liquid crystal (LC) molecules, while the film exhibits a transparent state result from the parallel alignment of N* phase LC molecules at a higher temperature. Importantly, the PSLC films with different temperature of phase transition and contrast ratio can be prepared by changing the composition of photo-polymerizable monomer/LC/chiral dopant. According to the competition between the polymerization of the curable monomers and the diffusion of LC molecules, the ultraviolet (UV) curing surrounding temperature and the intensity of UV irradiation play a critical role in tuning the size of the polymer network meshes, which in turn influence the contrast ratio and the switching speed of the film. Our observations are expected to pave the way for preparing smart PSLC thin films for applications in areas of smart windows, thermo-detectors and other information recording devices. (paper)

  18. The ortho backbone amide linker (o-BAL) is an easily prepared and highly acid-labile handle for solid-phase synthesis

    DEFF Research Database (Denmark)

    Boas, Ulrik; Brask, Jesper; Christensen, J.B.

    2002-01-01

    The tris(alkoxy)benzyl backbone amide linker (BAL) has found widespread application in solid-phase synthesis. The key intermediate for preparation of para BAL (p-BAL) is 2,6-dimethoxy-4-hydroxybenzaldehyde; several reports on its synthesis have appeared. However, the ortho analogue of the handle (o...

  19. Isolation and Purification of Unstable Iridoid Glucosides from Traditional Chinese Medicine by Preparative High Performance Liquid Chromatography Coupled with Solid-phase Extraction

    Institute of Scientific and Technical Information of China (English)

    LI Cun-man; XIAO Yuan-sheng; XUE Xing-ya; FENG Jia-tao; ZHANG Xiu-li; LIANG Xin-miao

    2011-01-01

    An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chro matography(HPLC) and solid-phase extraction(SPE). The aim of this study was to obtain an effective method with high preparative efficiency and importantly to avoid the transformation of unstable compounds. The preparative HPLC system was based on an LC/MS controlled four-channel autopurification system. The SPE method was per formed with a C1s packing material to trap the target compounds and to remove the acidic additive derived from the mobile phase. Using this method, the unstable iridoid glucosides(IGs) as model compounds were successfully iso lated and purified from the extract of Hedyotis diffusa Willd. Six IGs(including one new minor IG) and one nucleo tide compound were simultaneously obtained, each with a purity of >91% as determined by HPLC. The structures of the isolated compounds were identified by UPLC/Q-TOF MS, UV, ID and/or 2D NMR. It was demonstrated that the combination of preparative HPLC with SPE is a versatile tool for preparative purification of unstable compounds from complex natural products.

  20. Isolation and Purification of Unstable Iridoid Glucosides from Traditional Chinese Medicine by Preparative High Performance Liquid Chromatography Coupled with Solid-phase Extraction

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chro-matography(HPLC) and solid-phase extraction(SPE). The aim of this study was to obtain an effective method with high preparative efficiency and importantly to avoid the transformation of unstable compounds. The preparative HPLC system was based on an LC/MS controlled four-channel autopurification system. The SPE method was performed with a C18 packing material to trap the target compounds and to remove the acidic additive derived from the mobile phase. Using this method, the unstable iridoid glucosides(IGs) as model compounds were successfully isolated and purified from the extract of Hedyotis diffusa Willd. Six IGs(including one new minor IG) and one nucleotide compound were simultaneously obtained, each with a purity of 〉91% as determined by HPLC. The structures of the isolated compounds were identified by UPLC/Q-TOF MS, UV, 1D and/or 2D NMR. It was demonstrated that the combination of preparative HPLC with SPE is a versatile tool for preparative purification of unstable compounds from complex natural products.

  1. Study on preparation and thermal property of binary fatty acid and the binary fatty acids/diatomite composite phase change materials

    International Nuclear Information System (INIS)

    Li, Min; Kao, Hongtao; Wu, Zhishen; Tan, Jinmiao

    2011-01-01

    This study prepared a series of binary phase change materials by mixing decanoic acid, dodecanoic acid, hexadecanoic acid and octadecanoic acid each other. The phase-transition temperature of binary fatty acid and its corresponding mixing proportion are calculated with phase diagram thermodynamic method. The results are verified by the experimental result of the heat absorption curve and the Differential Scanning Calorimetry (DSC) analysis curve. The results show that the calculation method of phase diagram thermodynamic calculation can be taken as a basis for mixing proportion of binary fatty acid phase change materials. In addition, the decanoic-dodecanoic acid/diatomite composite phase change material (PCM) are prepared and its microstructure, thermal property and thermal reliability are characterized. The result shows that the decanoic-dodecanoic acid is uniformly adsorbed into diatomite and the form-stable PCM are formed. The phase-transition temperature and the latent heat of the decanoic-dodecanoic acid/diatomite composite PCMs is 16.74 o C and 66.8114 J/g, respectively.

  2. On the phase evolution of AlCoCrCuFeMnSix high entropy alloys prepared by mechanical alloying and arc melting route

    Science.gov (United States)

    Kumar, Anil; Chopkar, Manoj

    2018-05-01

    Effect of Si addition on phase formation of AlCoCrCuFeMnSix (x=0, 0.3, 0.6 and 0.9) high entropy alloy have been investigated in this work. The alloys are prepared by mechanical alloying and vacuum arc melting technique. The X-ray diffraction results reveals the formation of mixture of face centered and body centered cubic solid solution phases in milled powders. The addition of Si favours body centered cubic structure formation during milling process. Whereas, after melting the milled powders, body centered phases formed during milling is partial transformed into sigma phases. XRD results were also correlated with the SEM elemental mapping of as casted samples. Addition of Si favours σ phase formation in the as cast samples.

  3. A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

    International Nuclear Information System (INIS)

    Pelit, Füsun Okçu; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

    2015-01-01

    Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL −1 . Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues

  4. A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

    Energy Technology Data Exchange (ETDEWEB)

    Pelit, Füsun Okçu, E-mail: fusun.okcu@ege.edu.tr; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

    2015-02-15

    Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL{sup −1}. Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues.

  5. Two-step preparation of nano-scaled magnetic chitosan particles using Triton X-100 reversed-phase water-in-oil microemulsion system

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Zhengkun; Jiang, Feihong [College of Food Science and Engineering, Northwest A and F University, Yangling, Shaanxi 712100 (China); Lee, Tung-Ching, E-mail: lee@aesop.rutgers.edu [Department of Food Science, Rutgers, the State University of New Jersey, 65 Dudley Road, New Brunswick, NJ 08901 (United States); Yue, Tianli, E-mail: yuetl305@nwsuaf.edu.cn [College of Food Science and Engineering, Northwest A and F University, Yangling, Shaanxi 712100 (China)

    2013-12-25

    Highlights: •A new two-step route for nano-scaled magnetic chitosan particles preparation. •Triton X-100 reversed-phase microemulsion system was used for chitosan coating. •Narrow size distribution of magnetic chitosan nanoparticles was achieved. •Quantitative evaluation of recoverability for the magnetic chitosan nanoparticles. -- Abstract: A new two-step route for the preparation of nano-scaled magnetic chitosan particles has been developed, different from reported one-step in situ preparation and two-step preparation method of reversed-phase suspension, Triton X-100 reversed-phase water-in-oil microemulsion encapsulation method was employed in coating the pre-prepared Fe{sub 3}O{sub 4} nanoparticles with chitosan. The resultant magnetic chitosan particles owned a narrow size distribution ranging from 50 to 92 nm. X-ray diffraction patterns (XRD) indicated that the chitosan coating procedure did not change the spinal structure of Fe{sub 3}O{sub 4} magnetic nanoparticles. The results of Fourier transform infrared (FTIR) analysis and thermogravimetric analysis (TGA) demonstrated that the chitosan was coated on Fe{sub 3}O{sub 4} nanoparticles and its average mass content was ∼50%. The saturated magnetization of the magnetic Fe{sub 3}O{sub 4}/chitosan nanoparticles reached 18.62 emu/g, meanwhile, the nanoparticles showed the characteristics of superparamagnetism. The magnetic chitosan nanoparticles showed a high recoverability of 99.99% in 10 min when pH exceeded 4. The results suggested that the as-prepared magnetic chitosan particles were nano-scaled with a narrow size distribution and a high recoverability.

  6. Two-step preparation of nano-scaled magnetic chitosan particles using Triton X-100 reversed-phase water-in-oil microemulsion system

    International Nuclear Information System (INIS)

    Zhou, Zhengkun; Jiang, Feihong; Lee, Tung-Ching; Yue, Tianli

    2013-01-01

    Highlights: •A new two-step route for nano-scaled magnetic chitosan particles preparation. •Triton X-100 reversed-phase microemulsion system was used for chitosan coating. •Narrow size distribution of magnetic chitosan nanoparticles was achieved. •Quantitative evaluation of recoverability for the magnetic chitosan nanoparticles. -- Abstract: A new two-step route for the preparation of nano-scaled magnetic chitosan particles has been developed, different from reported one-step in situ preparation and two-step preparation method of reversed-phase suspension, Triton X-100 reversed-phase water-in-oil microemulsion encapsulation method was employed in coating the pre-prepared Fe 3 O 4 nanoparticles with chitosan. The resultant magnetic chitosan particles owned a narrow size distribution ranging from 50 to 92 nm. X-ray diffraction patterns (XRD) indicated that the chitosan coating procedure did not change the spinal structure of Fe 3 O 4 magnetic nanoparticles. The results of Fourier transform infrared (FTIR) analysis and thermogravimetric analysis (TGA) demonstrated that the chitosan was coated on Fe 3 O 4 nanoparticles and its average mass content was ∼50%. The saturated magnetization of the magnetic Fe 3 O 4 /chitosan nanoparticles reached 18.62 emu/g, meanwhile, the nanoparticles showed the characteristics of superparamagnetism. The magnetic chitosan nanoparticles showed a high recoverability of 99.99% in 10 min when pH exceeded 4. The results suggested that the as-prepared magnetic chitosan particles were nano-scaled with a narrow size distribution and a high recoverability

  7. Characterization of phase changes during fabrication of copper alloys, crystalline and non-crystalline, prepared by mechanical alloying

    Directory of Open Access Journals (Sweden)

    Paula Rojas

    2016-09-01

    Full Text Available The manufacture of alloys in solid state has many differences with the conventional melting (casting process. In the case of high energy milling or mechanical alloying, phase transformations of the raw materials are promoted by a large amount of energy that is introduced by impact with the grinding medium; there is no melting, but the microstructural changes go from microstructural refinement to amorphization in solid state. This work studies the behavior of pure metals (Cu and Ni, and different binary alloys (Cu-Ni and Cu-Zr, under the same milling/mechanical alloying conditions. After high-energy milling, X ray diffraction (XRD patterns were analyzed to determine changes in the lattice parameter and find both microstrain and crystallite sizes, which were first calculated using the Williamson-Hall (W-H method and then compared with the transmission electron microscope (TEM images. Calculations showed a relatively appropriate approach to observations with TEM; however, in general, TEM observations detect heterogeneities, which are not considered for the W-H method. As for results, in the set of pure metals, we show that pure nickel undergoes more microstrain deformations, and is more abrasive than copper (and copper alloys. In binary systems, there was a complete solid solution in the Cu-Ni system and a glass-forming ability for the Cu-Zr, as a function of the Zr content. Mathematical methods cannot be applied when the systems have amorphization because there are no equations representing this process during milling. A general conclusion suggests that, under the same milling conditions, results are very different due to the significant impact of the composition: nickel easily forms a solid solution, while with a higher zirconium content there is a higher degree of glassforming ability.

  8. Optimization of substrate preparation for oyster mushroom (Pleurotus ostreatus) cultivation by studying different raw materials and substrate preparation conditions (composting: phases I and II).

    Science.gov (United States)

    Vieira, Fabrício Rocha; de Andrade, Meire Cristina Nogueira

    2016-11-01

    In recent years, oyster mushroom (Pleurotus ostreatus) has become one of the most cultivated mushrooms in the world, mainly in Brazil. Among many factors involved in a mushroom production, substrate preparation is the most critical step, which can be influenced by composting management techniques. Looking forward to optimizing the substrate preparation process, were tested different composting conditions (7 and 14 days of composting with or without conditioning), potential raw materials (decumbens grass, brizantha grass and sugarcane straw) and nitrogen supplementation (with or without wheat bran) on oyster mushroom yield and biological efficiency (BE). The substrate composted for 7 days with conditioning showed higher yield and biological efficiency of mushroom (24.04 and 100.54 %, respectively). Substrates without conditioning (7 and 14 days of composting) showed smaller mushroom yield and biological efficiency. Among the raw materials tested, brizantha grass showed higher mushroom yield followed by decumbens grass, sugarcane straw and wheat straw (28.5, 24.32, 23.5 and 19.27 %, respectively). Brizantha grass also showed higher biological efficiency followed by sugarcane straw, decumbens grass and wheat straw (123.95, 103.70, 96.90 and 86.44 %, respectively). Supplementation with wheat bran improved yield and biological efficiency in all substrate formulations tested; thus, oyster mushroom yield and biological efficiency were influenced by substrate formulation (raw materials), supplementation and composting conditions.

  9. The Impact of Endurance Training on Functional Parameters During the Preparation Phase among Cross-Country Skiers

    Directory of Open Access Journals (Sweden)

    Žiška Peter

    2016-05-01

    Full Text Available In the study, we have tried to demonstrate the effect of endurance training on changes in functional parameters during the preparation phase (12-week mesocycle among cross-country skiers. The group consisted of 10 male cross-country skiers (age: 21.4 ±5 year who completed control (1st 6 week mesocycle and experimental period (2nd 6 week mesocycle.We focused on the following time-varying parameters: changes in maximal oxygen uptake (VO2max, the level of aerobic (AeT and anaerobic thresholds (AT, maximum heart rate (HRmax and performance on the running treadmill. The intra-individual monitoring of each athlete revealed statistical significance of VO2max (mid_VO2max = 69.48 ± 5.72 l.kg-1.min-1, post_ VO2max = 70.96 ± 5.67 ml.kg-1.min-1; p≤0.05 and the level of AT (mid_AT = 86.2 ± 5.43 %, post_AT = 87.8 ± 5.59 %; p≤0.01 the performance on the running treadmill (mid_t = 14:54 ± 1:43 min., post_t = 15:30 ± 1:50 min.; p≤0.05.The significant changes were recorded in the AeT(pre_AeT = 70.3 ± 7.56 %, mid_AeT = 72.5 ± 7.59 %; p≤0.05 in theHRmax(pre_HRmax = 190 ± 8.04 bpm, mid_HRmax = 189 bpm, post_HRmax = 188 ± 7.34 bpm; p = n.s. during control period. We assume that the significant differences occurred as a result of adaptation changes due to training stimuli, which were induced by changes in functional parameters. Increased training volume in zone lower level of oxygen regime (A1, upper level of oxygen regime (A2 and upper level of lactate tolerance(T2 during experimental period elicited changes which reflected the increase functional parameters and performance on the running treadmill compared to that of control period.

  10. Influence of the thermal regime of the multifilamentary wires preparation to the creation of the Nb/sub 3/Sn phase

    Energy Technology Data Exchange (ETDEWEB)

    Sitek, J.; Hucl, M.; Bajci, P.; Kruzliak, J.; Benacka, S.; Hut' ka, P.; Kovac, P.

    1984-06-01

    On the basis of the results obtained by Moessbauer spectroscopy and by measuring the critical temperature by means of the inductive method, the possibility of creating the Nb/sub 3/Sn phase in the composite filaments CuSn-Nb is discussed. The filaments were prepared by pressing at room temperature, and at temperatures of 550 to 600 deg C. Experimental details are given. Results are given and discussed.

  11. Preparation, microstructure and thermal properties of Mg−Bi alloys as phase change materials for thermal energy storage

    International Nuclear Information System (INIS)

    Fang, Dong; Sun, Zheng; Li, Yuanyuan; Cheng, Xiaomin

    2016-01-01

    Highlights: • The microstructure and thermal properties of Mg−Bi alloys are determined. • The relationship between melting enthalpies and phase composition are studied. • The activation energy of Mg−54%Bi alloy is calculated by multiple DSC technology. • Mg−54%Bi alloy is proposed as a phase change material at high (>420 °C) temperature. - Abstract: Comparing with Al-based phase change material, Mg-based phase change material is getting more and more attention due to its high corrosion resistance with encapsulation materials based on iron. This study focuses on the characterization of Mg−36%Bi, Mg−54%Bi and Mg−60%Bi (wt. %) alloys as phase change materials for thermal energy storage at high temperature. The phase compositions, microstructure and phase change temperatures were investigated by X-ray diffusion (XRD), electron probe micro-analysis (EPMA) and differential scanning calorimeter (DSC) analysis, respectively. The results indicates that the microstructure of Mg−36%Bi and Mg−54%Bi alloys are mainly composed of α-Mg matrix and α-Mg + Mg_3Bi_2 eutectic phases, Mg−60%Bi alloy are mainly composed of the Mg_3Bi_2 phase and α-MgMg_3Bi_2 eutectic phases. The melting enthalpies of Mg−36%Bi, Mg−54%Bi and Mg−60%Bi alloys are 138.2, 180.5 and 48.7 J/g, with the phase change temperatures of 547.6, 546.3 and 548.1 °C, respectively. The Mg−54%Bi alloy has the highest melting enthalpy in three alloys. The main reason may be that it has more proportion of α-Mg + Mg_3Bi_2 eutectic phases. The thermal expansion of three alloys increases with increasing temperature. The values of the thermal conductivity decrease with increasing Bi content. Besides, the activation energy of Mg−54%Bi was calculated by multiple DSC technology.

  12. Separation of four flavonol glycosides from Solanum rostratum Dunal using aqueous two-phase flotation followed by preparative high-performance liquid chromatography.

    Science.gov (United States)

    Chang, Lin; Shao, Qian; Xi, Xingjun; Chu, Qiao; Wei, Yun

    2017-02-01

    Aqueous two-phase flotation followed by preparative high-performance liquid chromatography was used to separate four flavonol glycosides from Solanum rostratum Dunal. In the aqueous two-phase flotation section, the effects of sublation solvent, solution pH, (NH 4 ) 2 SO 4 concentration in aqueous solution, cosolvent, N 2 flow rate, flotation time, and volumes of the polyethylene glycol phase on the recovery were investigated in detail, and the optimal conditions were selected: 50 wt% polyethylene glycol 1000 ethanol solvent as the flotation solvent, pH 4, 350 g/L of (NH 4 ) 2 SO 4 concentration in aqueous phase, 40 mL/min of N 2 flow rate, 30 min of flotation time, 10.0 mL of flotation solvent volume, and two times. After aqueous two-phase flotation concentration, the flotation products were purified by preparative high-performance liquid chromatography. The purities of the final products A and B were 98.1 and 99.0%. Product B was the mixture of three compounds based on the analysis of high-performance liquid chromatography at the temperature of 10°C, while product A was hyperoside after the identification by nuclear magnetic resonance. Astragalin, 3'-O-methylquercetin 3-O-β-d-galactopyranoside, and 3'-O-methylquercetin 3-O-β-d-glucopyranoside were obtained with the purity of 93.8, 97.1, and 99.2%, respectively, after the further separation of product B using preparative high-performance liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Preparation and thermal properties of Glauber’s salt-based phase-change materials for Qinghai-Tibet Plateau solar greenhouses

    Science.gov (United States)

    Jiang, Zipeng; Tie, Shengnian

    2017-07-01

    This paper reports the preparation and characterization of eutectic Glauber’s salt-based composite, phase-change materials (G-PCMs). PCMs were prepared using industrial-grade sodium sulfate decahydrate (Na2SO4 ṡ 10H2O) as the basic material. Other salts were added to obtain the eutectic Glauber’s salt-based PCMs with phase-change temperatures of 25∘C, 15∘C and 10∘C. The modification of the G-PCMs was designed using the same experimental method to select the efficient nucleating, thickening and thermal conductive agents. The results show that borax can be an effective nucleating agent, sodium carboxymethyl cellulose is an excellent thickener and carbon powder is a good thermal conductive agent. The phase-change temperature, latent heat and thermal conductivity of the three different PCMs are 23.9∘C, 15.4∘C and 9.5∘C; 179.6, 129 and 116.2 J/g; and 1.02, 1.10 and 1.23 W/(m K), respectively. These PCMs possess suitable phase-change temperature, high latent heat and good thermal conductivity, and can be used in Qinghai-Tibet Plateau agricultural solar greenhouses.

  14. Elimination of impurity phase formation in FePt magnetic thin films prepared by pulsed laser deposition

    International Nuclear Information System (INIS)

    Wang, Ying; Medwal, Rohit; Sehdev, Neeru; Yadian, Boluo; Tan, T.L.; Lee, P.; Talebitaher, A.; Ilyas, Usman; Ramanujan, R.V.; Huang, Yizhong; Rawat, R.S.

    2014-01-01

    The formation of impurity phases in FePt thin films severely degrades its magnetic properties. The X-ray diffraction patterns of FePt thin films, synthesized using pulsed laser deposition (PLD), showed peaks corresponding to impurity phases, resulting in softer magnetic properties. A systematic investigation was carried to determine the factors that might have led to impurity phase formation. The factors include (i) PLD target composition, (ii) substrate material, (iii) annealing parameters such as temperature, duration and ambience and (iv) PLD deposition parameters such as chamber ambience, laser energy fluence and target–substrate distance. Depositions on the different substrates revealed impurity phase formation only on Si substrates. It was found that the target composition, PLD chamber ambience, and annealing ambience were not the factors that caused the impurity phase formation. The annealing temperature and duration influenced the impurity phases, but are not the cause of their formation. A decrease in the laser energy fluence and increase of the target–substrate distance resulted in elimination of the impurity phases and enhancement in the magnetic and structural properties of FePt thin films. The energy of the ablated plasma species, controlled by the laser energy fluence and the target–substrate distance, is found to be the main factor responsible for the formation of the impurity phases.

  15. Phase transformation in sol-gel prepared zirconia using in-situ high temperature X-ray diffraction

    International Nuclear Information System (INIS)

    Srinivasan, R.; Davis, B.H.; Hubbard, C.R.; Cavin, O.B.; Porter, W.D.

    1991-01-01

    Zirconia was precipitated at a pH of 10.5 by admixing a solution of ZrCl 4 and NH 4 OH both rapidly (∼ 1 min) and slowly (∼ 8 hr). The precipitate was calcined at 500C for 5 hours and then furnace cooled. The former exhibited monoclinic phase while the latter yielded tetragonal phase. The pathway from amorphous to crystalline form was followed by in-situ high temperature X-ray diffraction in flowing air and in He. The data showed the evolution of the tetragonal crystalline phase on heating. On rapid cooling the tetragonal phase is retained at R.T., and on slow cooling the transformation to monoclinic phase occurs in air

  16. Releasing intracellular product to prepare whole cell biocatalyst for biosynthesis of Monascus pigments in water-edible oil two-phase system.

    Science.gov (United States)

    Hu, Minglue; Zhang, Xuehong; Wang, Zhilong

    2016-11-01

    Selective releasing intracellular product in Triton X-100 micelle aqueous solution to prepare whole cell biocatalyst is a novel strategy for biosynthesis of Monascus pigments, in which cell suspension culture exhibits some advantages comparing with the corresponding growing cell submerged culture. In the present work, the nonionic surfactant Triton X-100 was successfully replaced by edible plant oils for releasing intracellular Monascus pigments. High concentration of Monascus pigments (with absorbance nearly 710 AU at 470 nm in the oil phase, normalized to the aqueous phase volume approximately 142 AU) was achieved by cell suspension culture in peanut oil-water two-phase system. Furthermore, the utilization of edible oil as extractant also fulfills the demand for application of Monascus pigments as natural food colorant.

  17. Preparation and thermal characterization of oxalic acid dihydrate/bentonite composite as shape-stabilized phase change materials for thermal energy storage

    Science.gov (United States)

    Han, Lipeng; Xie, Shaolei; Sun, Jinhe; Jia, Yongzhong

    2017-03-01

    Oxalic acid dihydrate (OAD) which has very high initial phase transition enthalpy is a promising phase change material (PCM). In this paper, shape-stabilized composite PCMs composed of OAD and bentonite were prepared by a facile blending method to overcome the problem of leakage. FT-IR results indicated the interactions between OAD and bentonite, such as the capillary force and the hydrogen bonding, resulting in the confined crystallization process. As a result, the OAD was confined to be amorphous. The thermogravimetric analysis and scanning electron microscope results showed that sample had the best coating effect when the amount of bentonite was 17.7%. The differential scanning calorimetry analyses demonstrated that a decrease in the OAD content was accompanied by a continuous decrease in the melting point and phase change enthalpy of the composites.

  18. Preparation and characterization of hydrated salts/silica composite as shape-stabilized phase change material via sol–gel process

    International Nuclear Information System (INIS)

    Wu, Yuping; Wang, Tao

    2014-01-01

    Highlights: • A mixture of hydrated salts were adopted as phase change materials. • Phase segregation of the hydrated salts was inhibited. • Subcooling was slightly mitigated. • Thermal cycling performance was greatly improved after PVP coating. - Abstract: A novel shape-stabilized phase change material composite was prepared by impregnating the mixture of hydrated salts (Na 2 SO 4 ·10H 2 O–Na 2 HPO 4 ·12H 2 O) into porous silica matrix obtained by sol–gel process and further coated with polyvinylpyrrolidone (PVP) to improve the thermal cycling performance. The chemical compatibility, morphology and phase change properties were investigated by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), hot-stage polarizing optical microscope (HS-POM) and differential scanning calorimetry (DSC). Confined in the silica matrix, phase segregation of the hydrated salts was inhibited and subcooling was slightly mitigated. No leakage was observed during the solid–liquid phase transition even when the mass ratio of hydrated salts to silica was as high as 70:30. Results showed that the melting enthalpy of the composite can reach 106.2 kJ/kg with the melting temperature at 30.13 °C and there was no significant enthalpy loss after 30 thermal cycles

  19. Heterogeneous coarsening of Pb phase and the effect of Cu addition on it in a nanophase composite of Al-10 wt%Pb alloy prepared by mechanical alloying

    International Nuclear Information System (INIS)

    Zhu, M.; Liu, X.; Wu, Z.F.; Ouyang, L.Z.; Zeng, M.Q.

    2009-01-01

    A nanophase composite of Al-10 wt%Pb alloy was prepared by mechanical alloying. The coarsening behavior of Pb phase in the composite during heating process was investigated by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and nanoindentation test. The present work shows that the Pb phase grew substantially and had two different size distributions when the heating temperature was above 823 K. The different size distributions of Pb phase were owing to different grain size ranges of Al matrix in different regions, which led to the different growth rates of the Pb phase in those regions. It has been proposed that the different size ranges of Al grain appeared upon heating were originated from a statistical size distribution of Al grains in the as-milled powder. With the addition of a small amount of Cu, the heterogeneous growth of Pb phase can be suppressed, and the coarsening of Pb phase shows two distinct rates. This indicates that the coarsening is mainly governed by grain boundary diffusion and lattice diffusion of Al matrix in the initial stage and the later one, respectively

  20. Preparation and properties of lauric acid/silicon dioxide composites as form-stable phase change materials for thermal energy storage

    International Nuclear Information System (INIS)

    Fang Guiyin; Li Hui; Liu Xu

    2010-01-01

    Form-stable lauric acid (LA)/silicon dioxide (SiO 2 ) composite phase change materials were prepared using sol-gel methods. The LA was used as the phase change material for thermal energy storage, with the SiO 2 acting as the supporting material. The structural analysis of these form-stable LA/SiO 2 composite phase change materials was carried out using Fourier transformation infrared spectroscope (FT-IR). The microstructure of the form-stable composite phase change materials was observed by a scanning electronic microscope (SEM). The thermal properties and thermal stability were investigated by a differential scanning calorimeter (DSC) and a thermogravimetric analysis apparatus (TGA), respectively. The SEM results showed that the LA was well dispersed in the porous network of SiO 2 . The DSC results indicated that the melting latent heat of the form-stable composite phase change material is 117.21 kJ kg -1 when the mass percentage of the LA in the SiO 2 is 64.8%. The results of the TGA showed that these materials have good thermal stability. The form-stable composite phase change materials can be used for thermal energy storage in waste heat recovery and solar heating systems.

  1. Tuning crystal phase of NiS_x through electro-oxidized nickel foam: A novel route for preparing efficient electrocatalysts for oxygen evolution reaction

    International Nuclear Information System (INIS)

    Li, Xiao; Shang, Xiao; Rao, Yi; Dong, Bin; Han, Guan-Qun; Hu, Wen-Hui; Liu, Yan-Ru; Yan, Kai-Li; Chi, Jing-Qi; Chai, Yong-Ming; Liu, Chen-Guang

    2017-01-01

    Highlights: • Electro-oxidized nickel foam as a support has been used to prepare NiS_x phases. • Ni(OH)_2 layer on electro-oxidized NF is responsible for the growth of β-NiS. • NiS_x/NF(Ox) composed of β-NiS and Ni_3S_2 has enhanced electrocatalytic activity. • The growth mechanisms of mixed NiS_x phases of NiS_x/NF(Ox) have been discussed. - Abstract: A facile solvothermal sulfurization using electro-oxidized nickel foam (NF(Ox)) as support has been applied to prepare NiS_x/NF(Ox) electrocatalyst with highly efficient activity for oxygen evolution reaction (OER). XRD patterns confirm the composition of NiS_x/NF(Ox): two kinds of crystal phase including β-NiS and Ni_3S_2. While using bare NF as support under identical conditions, only Ni_3S_2 phase can be detected. SEM images reveal two kinds of morphologies of NiS_x/NF(Ox) including pyramids structure of β-NiS and nanorod-like structure of Ni_3S_2, which implies the tuning effect of electro-pretreatment of NF on the selective preparation of NiS_x crystal phase. It can be speculated that Ni(OH)_2 layer derived from electro-oxidized NF is responsible for the growth of β-NiS while metallic Ni is transformed into Ni_2S_3 during sulfurization. Electrochemical measurements for OER indicate the enhanced electrocatalytic activity of NiS_x/NF(Ox) with a small overpotential of 72 mV to reach 10 mA cm"−"2 compared with Ni_3S_2/NF, which may be ascribed to the improved electron-transfer kinetics relating to the unique atomic configurations and crystalline structures of β-NiS. The electro-oxidation pretreatment of nickel foam provides a simple and convenient method by tuning different NiS_x crystal phases for preparing excellent OER eletrocatalysts.

  2. Tuning crystal phase of NiS{sub x} through electro-oxidized nickel foam: A novel route for preparing efficient electrocatalysts for oxygen evolution reaction

    Energy Technology Data Exchange (ETDEWEB)

    Li, Xiao; Shang, Xiao [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); Rao, Yi [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); College of Science, China University of Petroleum (East China), Qingdao 266580, PR China (China); Dong, Bin, E-mail: dongbin@upc.edu.cn [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); College of Science, China University of Petroleum (East China), Qingdao 266580, PR China (China); Han, Guan-Qun [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); College of Science, China University of Petroleum (East China), Qingdao 266580, PR China (China); Hu, Wen-Hui; Liu, Yan-Ru; Yan, Kai-Li; Chi, Jing-Qi; Chai, Yong-Ming [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China); Liu, Chen-Guang, E-mail: cgliu@upc.edu.cn [State Key Laboratory of Heavy Oil Processing, China University of Petroleum (East China), Qingdao 266580 (China)

    2017-02-28

    Highlights: • Electro-oxidized nickel foam as a support has been used to prepare NiS{sub x} phases. • Ni(OH){sub 2} layer on electro-oxidized NF is responsible for the growth of β-NiS. • NiS{sub x}/NF(Ox) composed of β-NiS and Ni{sub 3}S{sub 2} has enhanced electrocatalytic activity. • The growth mechanisms of mixed NiS{sub x} phases of NiS{sub x}/NF(Ox) have been discussed. - Abstract: A facile solvothermal sulfurization using electro-oxidized nickel foam (NF(Ox)) as support has been applied to prepare NiS{sub x}/NF(Ox) electrocatalyst with highly efficient activity for oxygen evolution reaction (OER). XRD patterns confirm the composition of NiS{sub x}/NF(Ox): two kinds of crystal phase including β-NiS and Ni{sub 3}S{sub 2}. While using bare NF as support under identical conditions, only Ni{sub 3}S{sub 2} phase can be detected. SEM images reveal two kinds of morphologies of NiS{sub x}/NF(Ox) including pyramids structure of β-NiS and nanorod-like structure of Ni{sub 3}S{sub 2}, which implies the tuning effect of electro-pretreatment of NF on the selective preparation of NiS{sub x} crystal phase. It can be speculated that Ni(OH){sub 2} layer derived from electro-oxidized NF is responsible for the growth of β-NiS while metallic Ni is transformed into Ni{sub 2}S{sub 3} during sulfurization. Electrochemical measurements for OER indicate the enhanced electrocatalytic activity of NiS{sub x}/NF(Ox) with a small overpotential of 72 mV to reach 10 mA cm{sup −2} compared with Ni{sub 3}S{sub 2}/NF, which may be ascribed to the improved electron-transfer kinetics relating to the unique atomic configurations and crystalline structures of β-NiS. The electro-oxidation pretreatment of nickel foam provides a simple and convenient method by tuning different NiS{sub x} crystal phases for preparing excellent OER eletrocatalysts.

  3. The Combination Process for Preparative Separation and Purification of Paclitaxel and 10-Deacetylbaccatin III Using Diaion® Hp-20 Followed by Hydrophilic Interaction Based Solid Phase Extraction

    Science.gov (United States)

    Shirshekanb, Mahsa; Rezadoost, Hassan; Javanbakht, Mehran; Ghassempour, Ali Reza

    2017-01-01

    There is no other naturally occurring defense agent against cancer that has a stronger effect than paclitaxel, commonly known under the brand name of Taxol®. The major drawback for the more widespread use of paclitaxel and its precious precursor, 10-deacetylbaccatin III (10-DAB III), is that they require large-scale extraction from different parts of yew trees (Taxus species), cell cultures, taxane-producing endophytic fungi, and Corylus species. In our previous work, a novel online two-dimensional heart-cut liquid chromatography process using hydrophilic interaction/ reversed-phase chromatography was used to introduce a semi-preparative treatment for the separation of polar (10-deacetylbaccatin III) and non-polar (paclitaxel) taxanes from Taxus baccata L. In this work, a combination of the absorbent (Diaion® HP-20) and a silica based solid phase extraction is utilized as a new, efficient, and cost effective method for large-scale production of taxanes. This process avoids the technical problem of two-dimensional preparative liquid chromatography. The first stage of the process involves discarding co-extractive polar compounds including chlorophylls and pigments using a non-polar synthetic hydrophobic absorbent, Diaion® HP-20. Extract was then loaded on to a silica based hydrophilic interaction solid phase extraction (silica 40-60 micron). Taxanes was eluted using a mixture of water and methanol at the optimized ratio of 70:30. Finally, the fraction containing taxanes was applied to semi-preparative reversed phase HPLC. The results revealed that using this procedure, paclitaxel and 10-DAB III could be obtained at 8 and 3 times more, respectively than by the traditional method of extraction. PMID:29552048

  4. The Combination Process for Preparative Separation and Purification of Paclitaxel and 10-Deacetylbaccatin III Using Diaion® Hp-20 Followed by Hydrophilic Interaction Based Solid Phase Extraction.

    Science.gov (United States)

    Shirshekanb, Mahsa; Rezadoost, Hassan; Javanbakht, Mehran; Ghassempour, Ali Reza

    2017-01-01

    There is no other naturally occurring defense agent against cancer that has a stronger effect than paclitaxel, commonly known under the brand name of Taxol ® . The major drawback for the more widespread use of paclitaxel and its precious precursor, 10-deacetylbaccatin III (10-DAB III), is that they require large-scale extraction from different parts of yew trees ( Taxus species), cell cultures, taxane-producing endophytic fungi, and Corylus species. In our previous work, a novel online two-dimensional heart-cut liquid chromatography process using hydrophilic interaction/ reversed-phase chromatography was used to introduce a semi-preparative treatment for the separation of polar (10-deacetylbaccatin III) and non-polar (paclitaxel) taxanes from Taxus baccata L. In this work, a combination of the absorbent (Diaion ®  HP-20) and a silica based solid phase extraction is utilized as a new, efficient, and cost effective method for large-scale production of taxanes. This process avoids the technical problem of two-dimensional preparative liquid chromatography. The first stage of the process involves discarding co-extractive polar compounds including chlorophylls and pigments using a non-polar synthetic hydrophobic absorbent, Diaion ®  HP-20. Extract was then loaded on to a silica based hydrophilic interaction solid phase extraction (silica 40-60 micron). Taxanes was eluted using a mixture of water and methanol at the optimized ratio of 70:30. Finally, the fraction containing taxanes was applied to semi-preparative reversed phase HPLC. The results revealed that using this procedure, paclitaxel and 10-DAB III could be obtained at 8 and 3 times more, respectively than by the traditional method of extraction.

  5. Phase transformation and magnetic properties of MnAl powders prepared by elemental-doping and salt-assisted ball milling

    Science.gov (United States)

    Qian, Hui-Dong; Si, Ping-Zhan; Choi, Chul-Jin; Park, Jihoon; Cho, Kyung Mox

    2018-05-01

    The effects of elemental doping of Si and Fe on the ɛ→τ phase transformation and the magnetic properties of MnAl were studied. The magnetic powders of Si- and Fe-doped MnAl were prepared by using induction melting followed by water-quenching, annealing, and salt-assisted ball-milling. The Fe-doped MnAl powders are mainly composed of the L10-structured τ-phase, while the Si-doped MnAl are composed of τ-phase and a small fraction of γ2- and β-phases. A unique thin leaves-like morphology with thickness of several tens of nanometers and diameter size up to 500 nm were observed in the Si-doped MnAl powders. The Fe-doped MnAl powders show irregular shape with much larger dimensions in the range from several to 10 μm. The morphology difference of the samples was ascribed to the variation of the mechanical properties affected by different doping elements. The phase transformation temperatures of the ɛ-phase of the samples were measured. The doping of Fe decreases the onset temperature of the massive phase transformation in MnAl, while the Si-doping increases the massive phase transformation temperature. Both Fe and Si increase the Curie temperature of MnAl. A substantially enhanced coercivity up to 0.45 T and 0.42 T were observed in the ball-milled MnAl powders doped with Si and Fe, respectively.

  6. Design, preparation and application of a Pirkle-type chiral stationary phase for enantioseparation of some racemic organic acids and molecular dynamics studies

    Directory of Open Access Journals (Sweden)

    Reşit Çakmak

    2017-08-01

    Full Text Available This study consists of two parts. In the first part of the study; a Pirkle-type chiral stationary phase was prepared by synthesizing an aromatic amine derivative of (R-2-amino-1-butanol as a chiral selectorand binding to L- tyrosine -modified cyanogen bromide (CNBr-activated Sepharose 4B and then, packed into the separation column. T he chromatographic performance of the separation column was evaluated w ith racemic mandelic acid and 2-phenylpropionic acid by using phosphate buffers at three different pHs as mobile phase. In the resolution processes, t he prepared solutions were loaded onto the separation column at two different concentrations and at three different pHs for each racemic organic acid, separately. Enantiomeric excess (ee % of the eluates was determined on CHIRALPAK AD-H chiral analytical column by HPLC. The maximum ee% for mandelic acid and 2-phenylpropionic acid was determined to be 60.84 and 27.4, respectively. Separation factors (k 1 ’, k 2 ’, α, and Rs were calculated for each acid. The structures of the obtained compounds were characterized using the spectroscopic methods (NMR, and elemental analysis. In the second part of the study; enantioselective interactions between the prepared CSP and the analytes have been widely studied by docking, molecular dynamics simulation and quantum mechanical computation methods. The reason of column eluation of rac-2-phenylpropionic acid with lower enantiomeric yield was explained by these techniques.

  7. Chitosan-coated magnetic nanoparticles prepared in one-step by precipitation in a high-aqueous phase content reverse microemulsion.

    Science.gov (United States)

    Pineda, María Guadalupe; Torres, Silvia; López, Luis Valencia; Enríquez-Medrano, Francisco Javier; de León, Ramón Díaz; Fernández, Salvador; Saade, Hened; López, Raúl Guillermo

    2014-07-02

    Chitosan-coated magnetic nanoparticles (CMNP) were prepared in one-step by precipitation in a high-aqueous phase content reverse microemulsion in the presence of chitosan. The high-aqueous phase concentration led to productivities close to 0.49 g CMNP/100 g microemulsion; much higher than those characteristic of precipitation in reverse microemulsions for preparing magnetic nanoparticles. The obtained nanoparticles present a narrow particle size distribution with an average diameter of 4.5 nm; appearing to be formed of a single crystallite; furthermore they present superparamagnetism and high magnetization values; close to 49 emu/g. Characterization of CMNP suggests that chitosan is present as a non-homogeneous very thin layer; which explains the slight reduction in the magnetization value of CMNP in comparison with that of uncoated magnetic nanoparticles. The prepared nanoparticles show high heavy ion removal capability; as demonstrated by their use in the treatment of Pb2+ aqueous solutions; from which lead ions were completely removed within 10 min.

  8. Chitosan-Coated Magnetic Nanoparticles Prepared in One-Step by Precipitation in a High-Aqueous Phase Content Reverse Microemulsion

    Directory of Open Access Journals (Sweden)

    María Guadalupe Pineda

    2014-07-01

    Full Text Available Chitosan-coated magnetic nanoparticles (CMNP were prepared in one-step by precipitation in a high-aqueous phase content reverse microemulsion in the presence of chitosan. The high-aqueous phase concentration led to productivities close to 0.49 g CMNP/100 g microemulsion; much higher than those characteristic of precipitation in reverse microemulsions for preparing magnetic nanoparticles. The obtained nanoparticles present a narrow particle size distribution with an average diameter of 4.5 nm; appearing to be formed of a single crystallite; furthermore they present superparamagnetism and high magnetization values; close to 49 emu/g. Characterization of CMNP suggests that chitosan is present as a non-homogeneous very thin layer; which explains the slight reduction in the magnetization value of CMNP in comparison with that of uncoated magnetic nanoparticles. The prepared nanoparticles show high heavy ion removal capability; as demonstrated by their use in the treatment of Pb2+ aqueous solutions; from which lead ions were completely removed within 10 min.

  9. Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

    Science.gov (United States)

    Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

    2016-10-01

    In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Isotropic resolution diffusion tensor imaging of lumbosacral and sciatic nerves using a phase-corrected diffusion-prepared 3D turbo spin echo.

    Science.gov (United States)

    Cervantes, Barbara; Van, Anh T; Weidlich, Dominik; Kooijman, Hendrick; Hock, Andreas; Rummeny, Ernst J; Gersing, Alexandra; Kirschke, Jan S; Karampinos, Dimitrios C

    2018-08-01

    To perform in vivo isotropic-resolution diffusion tensor imaging (DTI) of lumbosacral and sciatic nerves with a phase-navigated diffusion-prepared (DP) 3D turbo spin echo (TSE) acquisition and modified reconstruction incorporating intershot phase-error correction and to investigate the improvement on image quality and diffusion quantification with the proposed phase correction. Phase-navigated DP 3D TSE included magnitude stabilizers to minimize motion and eddy-current effects on the signal magnitude. Phase navigation of motion-induced phase errors was introduced before readout in 3D TSE. DTI of lower back nerves was performed in vivo using 3D TSE and single-shot echo planar imaging (ss-EPI) in 13 subjects. Diffusion data were phase-corrected per k z plane with respect to T 2 -weighted data. The effects of motion-induced phase errors on DTI quantification was assessed for 3D TSE and compared with ss-EPI. Non-phase-corrected 3D TSE resulted in artifacts in diffusion-weighted images and overestimated DTI parameters in the sciatic nerve (mean diffusivity [MD] = 2.06 ± 0.45). Phase correction of 3D TSE DTI data resulted in reductions in all DTI parameters (MD = 1.73 ± 0.26) of statistical significance (P ≤ 0.001) and in closer agreement with ss-EPI DTI parameters (MD = 1.62 ± 0.21). DP 3D TSE with phase correction allows distortion-free isotropic diffusion imaging of lower back nerves with robustness to motion-induced artifacts and DTI quantification errors. Magn Reson Med 80:609-618, 2018. © 2018 The Authors Magnetic Resonance in Medicine published by Wiley Periodicals, Inc. on behalf of International Society for Magnetic Resonance in Medicine. This is an open access article under the terms of the Creative Commons Attribution NonCommercial License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited and is not used for commercial purposes. © 2018 The Authors Magnetic Resonance

  11. Characterization of Polyamide 66 membranes prepared by phase inversion using formic acid and hydrochloric acid such as solvents

    Directory of Open Access Journals (Sweden)

    Patrícia Poletto

    2011-12-01

    Full Text Available The membranes properties prepared from water/formic acid (FA/ polyamide 66 (PA66 and water/hydrochloric acid (HCl/polyamide 66 (PA 66 systems has been studied. The different solvents interact distinctly with the polymer, affecting the membrane morphology. The asymmetric structure of the membranes showed a dense top layer and a porous sublayer. The membranes M-HCl prepared from HCl/PA 66 system showed a larger dense layer (around 23 μm in compared to those prepared from FA/PA 66 system (M-FA (around 10 μm. The membrane morphology was a determinant factor in results of water absorption, porosity and pure water flux. The lower thickness of dense layer in M-FA membranes resulted in a higher water absorption and, consequently, porosity, approximately 50%, compared with M-HCl membranes, approximately 15%. The same trend was observed to permeate flux, the lower thickness of dense layer higher pure water flux.

  12. Preparation of Melamine - Formaldehyde Microcapsules Containing Hexadecane as a Phase Change Material: The Effect of Surfactants Type and Concentration

    Directory of Open Access Journals (Sweden)

    Zeinab Alinejad

    2013-05-01

    Full Text Available Microcapsules containing n-hexadecane (HD as the core and melamineformaldehyde (MF prepolymer as the shell were prepared by in-situ dispersion polymerization. The effects of surfactants type and amount were studied in relation to the morphology and thermal properties of microcapsules. The morphology of the microcapsules was studied using scanning electron microscopy (SEM and thermal properties were detected by differential scanning calorimetry (DSC and thermogravimetric analysis (TGA. SEM images showed that the increase in the amount of Triton X-100 (non-ionic to SDS (ionic ratio resulted in the agglomeration of the prepared microcapsules. This increase led also to lower encapsulated hexadecane and thermal stability of microcapsules. As a result, the optimum composition of the above surfactants for obtaining higher thermal stability and proper morphology wasfound to be 20 wt% of Triton X-100 and 80 wt% of SDS in the recipe. The optimum total amounts of surfactants was 4 wt%, which resulted in spherical and separate microcapsules. DSC and TGA analyses revealed that a sample prepared with 4 wt% of surfactants was not only successful in encapsulation of hexadecane but also showedhigher thermal stability compared with other formulations.

  13. Griffiths-like phase in high TC perovskite La2FeReO6 prepared in a controlled reducing atmosphere

    Science.gov (United States)

    Kaipamagalath, Aswathi; Palakkal, Jasnamol P.; Varma, Manoj R.

    2018-05-01

    The perovskite La2FeReO6 is prepared by solid-state reaction method. Calcination was done in a controlled reducing atmosphere. The structure of the compound is found to be orthorhombic with Pbnm space group. From the DC magnetic studies, the transition temperature (TC) of La2FeReO6 is found to be at 729 K. A Griffiths-like phase is present in the material with ferromagnetic short-range correlations above TC up to the Griffiths temperature TG = 863 K.

  14. Preparation of Nb-Si phases by cathode sputtering, in particulat the superconducting phase of epitactically grown A15-Nb3Si

    International Nuclear Information System (INIS)

    Siefken, U.

    1979-01-01

    The search for new superconducting materials with high transition temperatures is concentrated on alloys with a cubic A15 structure (Cr 3 Si structure). In this paper we present the preparation of metastable A15-Nb 3 Si which is expected to have a very high transition temperature Tsub(c). The properties of the A15 structure which are relevant for superconductivity are described, in particular the orthogonal chains as the most important structural characteristic, metastability, and the relation between lattice defects and transition temperature. For target compositions of 75% Nb / 25% Si and 80% Nb / 20% Si A15-Nb 3 Si transition temperatures of Tsub(c) = 5.3 K and Tsub(c) = 7.5 K have been measured respectively, with lattice constants asub(o) = 5.19 A and asub(o) = 5.18 A. (orig.) [de

  15. Preparation of peptide thioesters through fmoc-based solid-phase peptide synthesis by using amino thioesters

    DEFF Research Database (Denmark)

    Stuhr-Hansen, N.; Wilbek, T.S.; Strømgaard, K.

    2013-01-01

    protected peptide thioester, which was globally deprotected to afford the desired unprotected peptide thioester. The method is compatible with labile groups such as phosphoryl and glycosyl moieties. The synthesis of peptide alkyl thioesters by 9-fluorenylmethoxycarbonyl (Fmoc) solid-phase peptide synthesis...

  16. Creating Drug Solubilization Compartments via Phase Separation in Multicomponent Buccal Patches Prepared by Direct Hot Melt Extrusion-Injection Molding

    NARCIS (Netherlands)

    Alhijjaj, Muqdad; Bouman, Jacob; Wellner, Nikolaus; Belton, Peter; Qi, Sheng

    2015-01-01

    Creating in situ phase separation in solid dispersion based formulations to allow enhanced functionality of the dosage form, such as improving dissolution of poorly soluble model drug as well as being mucoadhesive, can significantly maximize the in vitro and in vivo performance of the dosage

  17. Advanced fabrication method for the preparation of MOF thin films: Liquid-phase epitaxy approach meets spin coating method.

    KAUST Repository

    Chernikova, Valeriya; Shekhah, Osama; Eddaoudi, Mohamed

    2016-01-01

    Here we report a new and advanced method for the fabrication of highly oriented/polycrystalline metal-organic framework (MOF) thin films. Building on the attractive features of the liquid-phase epitaxy (LPE) approach, a facile spin coating method

  18. Single-phase {beta}-FeSi{sub 2} thin films prepared on Si wafer by femtosecond laser ablation and its photoluminescence at room temperature

    Energy Technology Data Exchange (ETDEWEB)

    Lu Peixiang [State Key Laboratory of Laser Technology and Wuhan National Laboratory for Optoelectronics, Huazhong University of Science and Technology, Wuhan 430074 (China)]. E-mail: lupeixiang@mail.hust.edu.cn; Zhou Youhua [State Key Laboratory of Laser Technology and Wuhan National Laboratory for Optoelectronics, Huazhong University of Science and Technology, Wuhan 430074 (China) and Physics and Information School, Jianghan University, Wuhan 430056 (China)]. E-mail: yhzhou@jhun.edu.cn; Zheng Qiguang [State Key Laboratory of Laser Technology and Wuhan National Laboratory for Optoelectronics, Huazhong University of Science and Technology, Wuhan 430074 (China); Yang Guang [State Key Laboratory of Laser Technology and Wuhan National Laboratory for Optoelectronics, Huazhong University of Science and Technology, Wuhan 430074 (China)

    2006-02-06

    Single-phase {beta}-FeSi{sub 2} thin films were prepared on Si(100) and Si(111) wafers by using femtosecond laser deposition with a FeSi{sub 2} alloy target for the first time. X-ray diffraction (XRD), field scanning electron microscopy (FSEM), scanning probe microscopy (SPM), electron backscattered diffraction pattern (EBSD), and Fourier-transform Raman infrared spectroscopy (FTRIS) were used to characterize the structure, composition, and properties of the {beta}-FeSi{sub 2}/Si films. The orientation of {beta}-FeSi{sub 2} grains was found to depend on the orientation of the Si substrates, and photoluminescence at wavelength of 1.53 {mu}m was observed from the single-phase {beta}-FeSi{sub 2}/Si thin film at room temperature (20 {sup o}C)

  19. Phase-controlled preparation of TiO{sub 2} films and micro(nano)spheres by low-temperature chemical bath deposition

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Mingsong, E-mail: wangms@mail.ujs.edu.cn [School of Materials Science and Engineering, Jiangsu University, Zhenjiang 212013 (China); Li, Qihui; Yu, Haiyan [School of Materials Science and Engineering, Jiangsu University, Zhenjiang 212013 (China); Hur, Seung Hyun [Department of Chemical Engineering, University of Ulsan, Ulsan 680-749 (Korea, Republic of); Kim, Eui Jung, E-mail: ejkim@ulsan.ac.kr [Department of Chemical Engineering, University of Ulsan, Ulsan 680-749 (Korea, Republic of)

    2013-11-25

    Highlights: •Simultaneously preparation of TiO{sub 2} films and sphere-like precipitates by low-temperature chemical bath deposition. •The same building blocks observed in the films and precipitates. •Cluster-by-cluster attachment is succeeded by the ion-by-ion growth. •Phase-controlled growth of TiO{sub 2} by the effects of solvent or fluorine ion. -- Abstract: TiO{sub 2} films and micro(nano)spheres have been simultaneously prepared by means of low-temperature chemical bath deposition (CBD). The films and precipitates are found to be constructed of the same building blocks regardless of the bath conditions. Thin nanosheets of ca. 20 nm in thickness serve as the building blocks of rutile TiO{sub 2} grown in an acidic bath. They aggregate to form spheres to reduce the surface energy of the precipitates, while in the films they grow into discrete crystallites on the seeded substrate. Fine control over the crystalline phase of TiO{sub 2} is achieved by replacing some water with ethanol or the addition of NH{sub 4}F. A gradual transition from rutile to anatase is observed as the ethanol and NH{sub 4}F contents are increased. Moreover, the crystallite size of TiO{sub 2} is significantly reduced and there exists monodisperse nanoparticles and aggregate microspheres in the products modified with ethanol and NH{sub 4}F, respectively. This size-dependent phase transition is consistent with previous theoretical and thermodynamic studies. The facile tune of the TiO{sub 2} phase by low-temperature CBD method may be useful to improve the performance of TiO{sub 2} for its various applications.

  20. Identification of proteins in a human pleural exudate using two-dimensional preparative liquid-phase electrophoresis and matrix-assisted laser desorption/ionization mass spectrometry.

    Science.gov (United States)

    Nilsson, C L; Puchades, M; Westman, A; Blennow, K; Davidsson, P

    1999-01-01

    Pleural effusion may occur in patients suffering from physical trauma or systemic disorders such as infection, inflammation, or cancer. In order to investigate proteins in a pleural exudate from a patient with severe pneumonia, we used a strategy that combined preparative two-dimensional liquid-phase electrophoresis (2-D LPE), matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and Western blotting. Preparative 2-D LPE is based on the same principles as analytical 2-D gel electrophoresis, except that the proteins remain in liquid phase during the entire procedure. In the first dimension, liquid-phase isoelectric focusing allows for the enrichment of proteins in liquid fractions. In the Rotofor cell, large volumes (up to 55 mL) and protein amounts (up to 1-2 g) can be loaded. Several low abundance proteins, cystatin C, haptoglobin, transthyretin, beta2-microglobulin, and transferrin, were detected after liquid-phase isoelectric focusing, through Western blotting analysis, in a pleural exudate (by definition, >25 g/L total protein). Direct MALDI-TOF-MS analysis of proteins in a Rotofor fraction is demonstrated as well. MALDI-TOF-MS analysis of a tryptic digest of a continuous elution sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) fraction confirmed the presence of cystatin C. By applying 2-D LPE, MALDI-TOF-MS, and Western blotting to the analysis of this pleural exudate, we were able to confirm the identity of proteins of potential diagnostic value. Our findings serve to illustrate the usefulness of this combination of methods in the analysis of pathological fluids.

  1. Characterization of polymethyl methacrylate/polyethylene glycol/aluminum nitride composite as form-stable phase change material prepared by in situ polymerization method

    International Nuclear Information System (INIS)

    Zhang, Lei; Zhu, Jiaoqun; Zhou, Weibin; Wang, Jun; Wang, Yan

    2011-01-01

    Highlights: → Form-stable PMMA/PEG/AlN PCMs were prepared by in situ polymerization method. → AlN additive effectively enhanced the heat transfer property of composite PCMs. → The composites exhibited desirable thermal performance and electric insulativity. → The composites were available for the thermal management of electronic device. - Abstract: This work was focused on the preparation and characterization of a new type of form-stable phase change material (PCM) employed in thermal management. Using the method of in situ polymerization, polyethylene glycol (PEG) acting as the PCM and aluminum nitride (AlN) serving as the thermal conductivity promoter were uniformly encapsulated and embedded inside the three-dimensional network structure of PMMA matrix. When the mass fraction of PEG was below 70%, the prepared composite PCMs remained solid without leakage above the melting point of the PEG. XRD and FT-IR results indicated that the PEG was physically combined with PMMA matrix and AlN additive and did not participate in the polymerization. Thermal analysis results showed that the prepared composite PCMs possess available latent heat capacity and thermal stability, and the AlN additive was able to effectively enhance the heat transfer property of organic PCM. Moreover, the volume resistivity of composite achieved (5.92 ± 0.16) x 10 10 Ω cm when the mass ratio of AlN was 30%. To sum up, the prepared form-stable PCMs were competent for the thermal management of electronic device due to their acceptable thermal performance and electric insulativity.

  2. Study of the crystallographic phase change on copper (I) selenide thin films prepared through chemical bath deposition by varying the pH of the solution

    Energy Technology Data Exchange (ETDEWEB)

    Sandoval-Paz, M.G., E-mail: myrnasandoval@udec.cl [Departament of Physics, Faculty of Physical Sciences and Mathematics, University of Concepcion, Box 160-C, Concepción (Chile); Rodríguez, C.A. [Department of Materials Engineering, Faculty of Engineering, University of Concepción, Edmundo Larenas 270, Concepción 4070409 (Chile); Porcile-Saavedra, P.F. [Departament of Physics, Faculty of Physical Sciences and Mathematics, University of Concepcion, Box 160-C, Concepción (Chile); Trejo-Cruz, C. [Department of Physics, Faculty of Science, University of Biobío, Avenue Collao 1202, Box 5C, Concepción 4051381 (Chile)

    2016-07-15

    Copper (I) selenide thin films with orthorhombic and cubic structure were deposited on glass substrates by using the chemical bath deposition technique. The effects of the solution pH on the films growth and subsequently the structural, optical and electrical properties of the films were studied. Films with orthorhombic structure were obtained from baths wherein both metal complex and hydroxide coexist; while films with cubic structure were obtained from baths where the metal hydroxide there is no present. The structural modifications are accompanied by changes in bandgap energy, morphology and electrical resistivity of the films. - Graphical abstract: “Study of the crystallographic phase change on copper (I) selenide thin films prepared through chemical bath deposition by varying the pH of the solution” by M. G. Sandoval-Paz, C. A. Rodríguez, P. F. Porcile-Saavedra, C. Trejo-Cruz. Display Omitted - Highlights: • Copper (I) selenide thin films were obtained by chemical bath deposition. • Orthorhombic to cubic phase change was induced by varying the reaction solution pH. • Orthorhombic phase is obtained mainly from a hydroxides cluster mechanism. • Cubic phase is obtained mainly from an ion by ion mechanism. • Structural, optical and electrical properties are presented as a function of pH.

  3. Structure and phase transition of BiFeO{sub 3} cubic micro-particles prepared by hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Jian-Ping, E-mail: zhoujp@snnu.edu.cn [College of Physics and Information Technology, Shaanxi Normal University, Xi’an 710062 (China); Yang, Ruo-Lin; Xiao, Rui-Juan; Chen, Xiao-Ming [College of Physics and Information Technology, Shaanxi Normal University, Xi’an 710062 (China); Deng, Chao-Yong [Department of Electronic Science, Guizhou University, Guizhou Guiyang 550025 (China)

    2012-11-15

    Graphical abstract: Bismuth ferrite (BiFeO{sub 3}) cubic micro-particles with smooth surfaces were synthesized. BiFeO{sub 3} has a hexagonal perovskite structure with a space group R3c below 370 °C and rhombohedral perovskite structure with a space group R3m below 755 °C, undergoes a phase transition in the temperature range of 755–817 °C to a cubic structure, then decompose to liquid and Fe{sub 2}O{sub 3} above 939 °C. Highlights: ► BiFeO{sub 3} micro-particles with smooth surface were synthesized by hydrothermal method. ► BiFeO{sub 3} enjoys hexagonal structure with well element ratio and chemical valence. ► BiFeO{sub 3} transition from rhombohedral phase to cubic phase lasts 60 °C. -- Abstract: Single-phase bismuth ferrite (BiFeO{sub 3}) powders were synthesized with a hydrothermal method by controlling the experimental conditions carefully. The powder structure, morphology and composition were characterized by using X-ray diffraction (XRD), scanning electron microscopy, transmission electron microscope, Raman measurement and X-ray photoelectron spectroscopy. The particles change from irregular agglomerations to regular cubes with increasing KOH concentration. The large BiFeO{sub 3} cubic particles enjoy much smooth surfaces with well-matched element ratio (Bi:Fe:O = 1:1:3) and chemical valence (Bi{sup 3+}, Fe{sup 3+} and O{sup 2−}). The high temperature XRD and differential scanning calorimetry show that BiFeO{sub 3} powders have a hexagonal perovskite structure with a space group R3c below 370 °C and a rhombohedral structure with a space group R3m below 755 °C. BiFeO{sub 3} undergoes a phase transition in the temperature range of 755–817 °C from rhombohedral structure to a cubic phase, then decomposes to liquid and Fe{sub 2}O{sub 3} above 939 °C.

  4. Structure and phase transition of BiFeO3 cubic micro-particles prepared by hydrothermal method

    International Nuclear Information System (INIS)

    Zhou, Jian-Ping; Yang, Ruo-Lin; Xiao, Rui-Juan; Chen, Xiao-Ming; Deng, Chao-Yong

    2012-01-01

    Graphical abstract: Bismuth ferrite (BiFeO 3 ) cubic micro-particles with smooth surfaces were synthesized. BiFeO 3 has a hexagonal perovskite structure with a space group R3c below 370 °C and rhombohedral perovskite structure with a space group R3m below 755 °C, undergoes a phase transition in the temperature range of 755–817 °C to a cubic structure, then decompose to liquid and Fe 2 O 3 above 939 °C. Highlights: ► BiFeO 3 micro-particles with smooth surface were synthesized by hydrothermal method. ► BiFeO 3 enjoys hexagonal structure with well element ratio and chemical valence. ► BiFeO 3 transition from rhombohedral phase to cubic phase lasts 60 °C. -- Abstract: Single-phase bismuth ferrite (BiFeO 3 ) powders were synthesized with a hydrothermal method by controlling the experimental conditions carefully. The powder structure, morphology and composition were characterized by using X-ray diffraction (XRD), scanning electron microscopy, transmission electron microscope, Raman measurement and X-ray photoelectron spectroscopy. The particles change from irregular agglomerations to regular cubes with increasing KOH concentration. The large BiFeO 3 cubic particles enjoy much smooth surfaces with well-matched element ratio (Bi:Fe:O = 1:1:3) and chemical valence (Bi 3+ , Fe 3+ and O 2− ). The high temperature XRD and differential scanning calorimetry show that BiFeO 3 powders have a hexagonal perovskite structure with a space group R3c below 370 °C and a rhombohedral structure with a space group R3m below 755 °C. BiFeO 3 undergoes a phase transition in the temperature range of 755–817 °C from rhombohedral structure to a cubic phase, then decomposes to liquid and Fe 2 O 3 above 939 °C.

  5. Dense and high-stability Ti2AlN MAX phase coatings prepared by the combined cathodic arc/sputter technique

    Science.gov (United States)

    Wang, Zhenyu; Liu, Jingzhou; Wang, Li; Li, Xiaowei; Ke, Peiling; Wang, Aiying

    2017-02-01

    Ti2AlN belongs to a family of ternary nano-laminate alloys known as the MAX phases, which exhibit a unique combination of metallic and ceramic properties. In the present work, the dense and high-stability Ti2AlN coating has been successfully prepared through the combined cathodic arc/sputter deposition, followed by heat post-treatment. It was found that the as-deposited Ti-Al-N coating behaved a multilayer structure, where (Ti, N)-rich layer and Al-rich layer grew alternately, with a mixed phase constitution of TiN and TiAlx. After annealing at 800 °C under vacuum condition for 1.5 h, although the multilayer structure still was found, part of multilayer interfaces became indistinct and disappeared. In particular, the thickness of the Al-rich layer decreased in contrast to that of as-deposited coating due to the inner diffusion of the Al element. Moreover, the Ti2AlN MAX phase emerged as the major phase in the annealed coatings and its formation mechanism was also discussed in this study. The vacuum thermal analysis indicated that the formed Ti2AlN MAX phase exhibited a high-stability, which was mainly benefited from the large thickness and the dense structure. This advanced technique based on the combined cathodic arc/sputter method could be extended to deposit other MAX phase coatings with tailored high performance like good thermal stability, high corrosion and oxidation resistance etc. for the next protective coating materials.

  6. Preparation and Performance Analysis of Na2SO4·10H2O/EG Composite Phase-change Materials

    Directory of Open Access Journals (Sweden)

    LENG Cong-bin

    2017-01-01

    Full Text Available Sodium sulfate decahydrate/expanded graphite composite phase-change material (Na2SO4·10H2O/EG was prepared by vacuum adsorption method.The thermal properties of Na2SO4·10H2O/EG,such as melting-solidification,phase separation,supercooling and latent heat were tested and analyzed.The results show that with the addition of 2%(mass fraction borax and 8% EG,the composite phase-change materials Na2SO4·10H2O/EG obtain ideal properties.The phase separation is eliminated,the supercooling degree of Na2SO4·10H2O is reduced from 13.6℃ to below 0.6℃,the latent heat and the energy storage density of the phase-change materials reach 225.77kJ·kg-1 and 218.09MJ·m-3 respectively.The thermal conductivity is also greatly improved.Compared with Na2SO4·10H2O with the addition of the nucleating agent borax only,the time for heat storage is shortened by 52.6%,and the time for heat release is shortened by 55.1%.Even after 500 times of rapid heating and cooling cycles,the performance of Na2SO4·10H2O/EG does not deteriorate.The novel composite phase-change material has better storage/exothermic properties.

  7. Influence of compaction pressure on the morphology and phase evolution of porous NiTi alloy prepared by SHS technique

    Directory of Open Access Journals (Sweden)

    Sirikul Wisutmethangoon

    2008-08-01

    Full Text Available The influence of compaction pressure on the pore morphology of porous NiTi shape memory alloys (SMAs fabricated by self-propagating high-temperature synthesis (SHS was investigated. The compaction pressure has a significant effect on the combustion temperature and pore morphology. The porous NiTi (SMAs thus obtained have the porosity of product in the range of 37.4-57.9 vol.%. The open porosity ratios were observed to be greater than 88%, which indicatesthat porous NiTi (SMAs are suitable for biomedical applications. In addition, the predominant phases in the porous product are B2(NiTi and B19’(NiTi with small amounts of secondary phases, NiTi2 and Ni4Ti3.

  8. Complexation induced phase separation: preparation of composite membranes with a nanometer thin dense skin loaded with metal ions

    KAUST Repository

    Villalobos Vazquez de la Parra, Luis Francisco

    2015-04-21

    We present the development of a facile phase-inversion method for forming asymmetric membranes with a precise high metal ion loading capacity in only the dense layer. The approach combines the use of macromolecule-metal intermolecular complexes to form the dense layer of asymmetric membranes with nonsolvent-induced phase separation to form the porous support. This allows the independent optimization of both the dense layer and porous support while maintaining the simplicity of a phase-inversion process. Moreover, it facilitates control over (i) the thickness of the dense layer throughout several orders of magnitude—from less than 15 nm to more than 6 μm, (ii) the type and amount of metal ions loaded in the dense layer, (iii) the morphology of the membrane surface, and (iv) the porosity and structure of the support. This simple and scalable process provides a new platform for building multifunctional membranes with a high loading of well-dispersed metal ions in the dense layer.

  9. Impact of concentration and Si doping on the properties and phase transformation behavior of nanocrystalline alumina prepared via solvothermal synthesis

    International Nuclear Information System (INIS)

    Mekasuwandumrong, Okorn; Tantichuwet, Panutin; Chaisuk, Choowong; Praserthdam, Piyasan

    2008-01-01

    Solvothermal reaction of 20 g aluminum isopropoxide (AIP) in mineral oil at 300 deg. C for 2 h gave χ-alumina showing high thermal stability while the reaction with higher amounts of starting AIP (30 and 40 g) contributed contamination of pseudoboehmite. The χ-alumina thus obtained directly transformed into α-alumina completely at approximately 1400 deg. C bypassing the other transition alumina phases whereas some part of the contaminated product transformed to γ-alumina through θ-alumina and finally α-alumina. When silicon was doped in the alumina matrix (5, 10, 20 and 50 at.%) using tetraethylorthosilicate as the silicon (Si) precursor, χ-alumina was still observed without any contaminations at low concentration doping (5-20 at.%). Amorphous structure was obtained by doping 50 at.% Si. The phase transformation temperature was shifted to the high temperature after loading the Si. The α-phase transformation did not go to completion even after calcinations at 1500 deg. C. This could be due to the incorporation of Si atom in alumina lattice forming SiO 2 -Al 2 O 3 solid solution

  10. Complexation induced phase separation: preparation of composite membranes with a nanometer thin dense skin loaded with metal ions

    KAUST Repository

    Villalobos Vazquez de la Parra, Luis Francisco; Karunakaran, Madhavan; Peinemann, Klaus-Viktor

    2015-01-01

    We present the development of a facile phase-inversion method for forming asymmetric membranes with a precise high metal ion loading capacity in only the dense layer. The approach combines the use of macromolecule-metal intermolecular complexes to form the dense layer of asymmetric membranes with nonsolvent-induced phase separation to form the porous support. This allows the independent optimization of both the dense layer and porous support while maintaining the simplicity of a phase-inversion process. Moreover, it facilitates control over (i) the thickness of the dense layer throughout several orders of magnitude—from less than 15 nm to more than 6 μm, (ii) the type and amount of metal ions loaded in the dense layer, (iii) the morphology of the membrane surface, and (iv) the porosity and structure of the support. This simple and scalable process provides a new platform for building multifunctional membranes with a high loading of well-dispersed metal ions in the dense layer.

  11. Visit at CERN of representatives of the Department of Piacenza (Italy), received by Lucio Rossi and Ugo Amaldi and hosted by the DG. The department of Piacenza is the native land of Edoardo Amaldi, one of the founding fathers of CERN, and the Department is preparing the celebration of the centennial of his birth.

    CERN Multimedia

    Maximilien Brice

    2008-01-01

    Visit at CERN of representatives of the Department of Piacenza (Italy), received by Lucio Rossi and Ugo Amaldi and hosted by the DG. The department of Piacenza is the native land of Edoardo Amaldi, one of the founding fathers of CERN, and the Department is preparing the celebration of the centennial of his birth.

  12. Effects of chronic exposure to low-level pollutants in the environment. Prepared for the Subcommittee on the Environment and the Atmosphere of the Committee on Science and Technology, US House of Representatives, Ninety-Fourth Congress, First Session by the Congressional Research Service, Library of Congress, Serial 0

    Energy Technology Data Exchange (ETDEWEB)

    1975-01-01

    This report was prepared for the Subcommittee on the Environment and the Atmosphere of the US House of Representatives Committee on Science and Technology. It describes the effects of low-level, persistent pollutants on human health, fish and wildlife, agriculture, and climate.

  13. Education and Job Training: Preparing for the 21st Century Workforce. Hearing before the Subcommittee on 21st Century Competitiveness of the Committee on Education and the Workforce, House of Representatives. One Hundred Seventh Congress, Second Session (Angola, Indiana, March 22, 2002).

    Science.gov (United States)

    Congress of the U.S., Washington, DC. House Committee on Education and the Workforce.

    This is a congressional hearing on how vocational and technical education and job training work together to better prepare workers for the 21st century workforce and on successful educational and job training activities and initiatives in Indiana (IN). Testimony includes statements from United States representatives (Howard P. "Buck"…

  14. A series of spinel phase cathode materials prepared by a simple hydrothermal process for rechargeable lithium batteries

    International Nuclear Information System (INIS)

    Liang Yanyu; Bao Shujuan; Li Hulin

    2006-01-01

    A series of spinel-structured materials have been prepared by a simple hydrothermal procedure in an aqueous medium. The new synthetic method is time and energy saving i.e., no further thermal treatment and extended grinding. The main experimental process involved the insertion of lithium into electrolytic manganese dioxide with glucose as a mild reductant in an autoclave. Both the hydrothermal temperature and the presence of glucose play the critical roles in determining the final spinel integrity. Particular electrochemical performance has also been systematically explored, and the results show that Al 3+ , F - co-substituted spinels have the best combination of initial capacity and capacity retention among all these samples, exhibited the initial capacity of 115 mAh/g and maintained more than 90% of the initial value at the 50th cycle. - Graphical abstract: It is a SEM image of the spinel LiMn 2 O 4 , which was prepared by this novel hydrothermal procedure. It illustrates that reasonable-crystallized spinel oxide has occurred through the special hydrothermal process and the average particle size declined to about 1 μm. This homogeneous grain size distribution provides an important morphological basis for the reversibility and accessibility of lithium ion insertion/extraction reactions

  15. Preparation of LuAG Powders with Single Phase and Good Dispersion for Transparent Ceramics Using Co-Precipitation Method

    Science.gov (United States)

    Pan, Liangjie; Jiang, Benxue; Fan, Jintai; Yang, Qiuhong; Zhou, Chunlin; Zhang, Pande; Mao, Xiaojian; Zhang, Long

    2015-01-01

    The synthesis of pure and well dispersed lutetium aluminum garnet (LuAG) powder is crucial and important for the preparation of LuAG transparent ceramics. In this paper, high purity and well dispersed LuAG powders have been synthesized via co-precipitation method with lutetium nitrate and aluminum nitrate as raw materials. Ammonium hydrogen carbonate (AHC) was used as the precipitant. The influence of aging time, pH value, and dripping speed on the prepared LuAG powders were investigated. It showed that long aging duration (>15 h) with high terminal pH value (>7.80) resulted in segregation of rhombus Lu precipitate and Al precipitate. By decreasing the initial pH value or accelerating the dripping speed, rhombus Lu precipitate was eliminated and pure LuAG nano powders were synthesized. High quality LuAG transparent ceramics with transmission >75% at 1064 nm were fabricated using these well dispersed nano LuAG powders. PMID:28793510

  16. Preparation of LuAG Powders with Single Phase and Good Dispersion for Transparent Ceramics Using Co-Precipitation Method

    Directory of Open Access Journals (Sweden)

    Liangjie Pan

    2015-08-01

    Full Text Available The synthesis of pure and well dispersed lutetium aluminum garnet (LuAG powder is crucial and important for the preparation of LuAG transparent ceramics. In this paper, high purity and well dispersed LuAG powders have been synthesized via co-precipitation method with lutetium nitrate and aluminum nitrate as raw materials. Ammonium hydrogen carbonate (AHC was used as the precipitant. The influence of aging time, pH value, and dripping speed on the prepared LuAG powders were investigated. It showed that long aging duration (>15 h with high terminal pH value (>7.80 resulted in segregation of rhombus Lu precipitate and Al precipitate. By decreasing the initial pH value or accelerating the dripping speed, rhombus Lu precipitate was eliminated and pure LuAG nano powders were synthesized. High quality LuAG transparent ceramics with transmission >75% at 1064 nm were fabricated using these well dispersed nano LuAG powders.

  17. Physical-chemical and technological aspects of the preparation of think layers of the high temperature superconductors Bi-Sr-Ca-Cu-O by method of metal organic vapour phase epitaxy

    International Nuclear Information System (INIS)

    Stejskal, J.; Nevriva, M.; Leitner, J.

    1995-01-01

    The method of metal organic vapour phase epitaxy (MO VPE) was used for preparation of think layers of the high temperature superconductors Bi-Sr-Ca-Cu-O. The suitable chemical precursors (β-diketonates) on the literature data and of the own thermodynamic calculations were selected. The optimal thermodynamic data and thermodynamic stability of the prepared samples were determined

  18. Solvent-assisted dispersive solid-phase extraction: A sample preparation method for trace detection of diazinon in urine and environmental water samples.

    Science.gov (United States)

    Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

    2016-09-02

    In this research, a sample preparation method termed solvent-assisted dispersive solid-phase extraction (SA-DSPE) was applied. The used sample preparation method was based on the dispersion of the sorbent into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was received by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the diazinon, the cloudy solution was centrifuged and diazinon in the sediment phase dissolved in ethanol and determined by gas chromatography-flame ionization detector. Under the optimized conditions (pH of solution=7.0, Sorbent: benzophenone, 2%, Disperser solvent: ethanol, 500μL, Centrifuge: centrifuged at 4000rpm for 3min), the method detection limit for diazinon was 0.2, 0.3, 0.3 and 0.3μgL(-1) for distilled water, lake water, waste water and urine sample, respectively. Furthermore, the pre-concentration factor was 363.8, 356.1, 360.7 and 353.38 in distilled water, waste water, lake water and urine sample, respectively. SA-DSPE was successfully used for trace monitoring of diazinon in urine, lake and waste water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Preparation and properties of shape-stabilized phase change materials based on fatty acid eutectics and cellulose composites for thermal energy storage

    International Nuclear Information System (INIS)

    Cao, Lei; Tang, Yaojie; Fang, Guiyin

    2015-01-01

    Shape-stabilized fatty acid eutectics/carboxy methyl cellulose-1 composites as phase change materials (PCMs) were synthesized by absorbing liquid eutectics into the carboxy methyl cellulose-1 fibers. The chemical structure, crystalloid phase and morphology were determined by the Fourier transformation infrared spectroscope, X-ray diffractometer and scanning electronic microscope. The thermal properties and thermal stability were measured by the differential scanning calorimeter, thermogravimetric analyzer and the thermal cycling test, respectively. The results indicate that the eutectics are well adsorbed in the porous structure of the carboxy methyl cellulose-1. According to the DSC (differential scanning calorimeter) results, the composites melt at 32.2 °C with latent heat of 114.6 kJ/kg and solidify at 29.2 °C with latent heat of 106.8 kJ/kg. The thermal cycling test proves that the composites have good thermal reliability. It is envisioned that the prepared shape-stabilized PCMs have considerable potential for developing their roles in thermal energy storage. - Highlights: • The fatty acid eutectic/carboxy methyl cellulose-1 composites as PCMs were prepared. • Chemical structure and microstructure of composites were determined by FT-IR and SEM. • Thermal properties and stabilities were investigated by DSC and TGA. • The thermal cycling test confirmed that the composite has good thermal reliability

  20. Preparation of acryloyl β-cyclodextrin-silica hybrid monolithic column and its application in pipette tip solid-phase extraction and HPLC analysis of methyl parathion and fenthion.

    Science.gov (United States)

    Chen, Ling; Dang, Xueping; Ai, Youhong; Chen, Huaixia

    2018-05-07

    An acryloyl β-cyclodextrin-silica hybrid monolithic column for pipette tip solid-phase extraction and high-performance liquid chromatography determination of methyl parathion and fenthion have been prepared through a sol-gel polymerization method. The synthesis conditions, including the volume of cross-linker and the ratio of inorganic solution to organic solution, were optimized. The prepared monolithic column was characterized by thermogravimetric analysis, scanning electron microscopy and Fourier transform infrared spectroscopy. The eluent type, volume and flow rate, sample volume, flow rate, acidity and ionic strength were optimized in detail. Under the optimized conditions, a simple and sensitive pipette tip solid-phase extraction with high-performance liquid chromatography method was developed for the determination of methyl parathion and fenthion in lettuce. The method yielded a linear calibration curve in the concentration ranges of 15-400 μg/kg for methyl parathion and 20-400 μg/kg for fenthion with correlation coefficients of above 0.9957. The limits of detection were 4.5 μg/kg for methyl parathion and 6.0 μg/kg for fenthion, respectively. The recoveries of methyl parathion and fenthion spiked in lettuce ranged from 96.0 to 104.2% with relative standard deviations less than 8.4%. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  1. A solid-phase technique for preparation of no-carrier-added technetium-99m radiopharmaceuticals: application to the streptavidin/biotin system

    International Nuclear Information System (INIS)

    Dunn-Dufault, Robert; Pollak, Alfred; Fitzgerald, Jane; Thornback, John R.; Ballinger, James R.

    2000-01-01

    A high effective specific activity (HESA) formulation of a biotin-containing 99m Tc ligand [RP488: dimethyl-Gly-Ser-Cys(Acm)-Lys(Biotin)-Gly] conveniently prepared from solid phase was compared to a typical low effective specific activity (LESA) solution formulation to demonstrate improved targeting to streptavidin in an in vitro assay and in an in vivo rat model. RP488 was coupled to a maleimide-functionalized polyethylene glycol resin via a thiol ether linkage and labeled with 99m Tc-gluconate at room temperature, followed by elution of the HESA 99m Tc-RP488 in saline (minimum specific activity ∼ 1000 TBq/mmol by amino acid analysis). Both HESA and LESA 99m Tc-RP488 labeled at > 90% purity. In vitro, HESA 99m Tc-RP488 incubated with streptavidin-agarose was bound quantitatively, but there was competition from addition of increasing amounts of cold RP488. In rats, radiotracer uptake was evident at the site of implantation of streptavidin-agarose beads for the HESA dose, less uptake of low effective specific activity (LESA) material, and no appreciable uptake in the control rats of the LESA or HESA dose. The target-to-background ratio for HESA 99m Tc-RP488 was 5.4 times that of the control. The solid-phase technology offers a convenient way to prepare high specific activity receptor-targeting 99m Tc radiopharmaceuticals

  2. THE JUNIOR COLLEGE AND EDUCATION IN THE SCIENCES. THIRD REPORT IN A SERIES PREPARED FOR THE SUBCOMMITTEE ON SCIENCE, RESEARCH, AND DEVELOPMENT OF THE COMMITTEE ON SCIENCE AND ASTRONAUTICS OF THE U.S. HOUSE OF REPRESENTATIVES. (TITLE SUPPLIED).

    Science.gov (United States)

    HAWORTH, LELAND J.

    THIS THIRD REPORT ON SCIENCE EDUCATION IN THE U.S. RAISES THREE ISSUES FOR THE JUNIOR COLLEGE--(1) IS IT A DISCRETE RESOURCE IN THE ADVANCEMENT OF SCIENCE EDUCATION, (2) DOES IT REQUIRE A UNIQUE SCIENCE CURRICULUM, AND (3) HOW SHOULD ITS SCIENCE INSTRUCTORS BE PREPARED. UNDER THE COUNCIL OF STATE GOVERNMENTS'"MODEL LAW" (1965), THE COMPREHENSIVE,…

  3. Development and optimization of a novel sample preparation method cored on functionalized nanofibers mat-solid-phase extraction for the simultaneous efficient extraction of illegal anionic and cationic dyes in foods.

    Science.gov (United States)

    Qi, Feifei; Jian, Ningge; Qian, Liangliang; Cao, Weixin; Xu, Qian; Li, Jian

    2017-09-01

    A simple and efficient three-step sample preparation method was developed and optimized for the simultaneous analysis of illegal anionic and cationic dyes (acid orange 7, metanil yellow, auramine-O, and chrysoidine) in food samples. A novel solid-phase extraction (SPE) procedure based on nanofibers mat (NFsM) was proposed after solvent extraction and freeze-salting out purification. The preferred SPE sorbent was selected from five functionalized NFsMs by orthogonal experimental design, and the optimization of SPE parameters was achieved through response surface methodology (RSM) based on the Box-Behnken design (BBD). Under the optimal conditions, the target analytes could be completely adsorbed by polypyrrole-functionalized polyacrylonitrile NFsM (PPy/PAN NFsM), and the eluent was directly analyzed by high-performance liquid chromatography-diode array detection (HPLC-DAD). The limits of detection (LODs) were between 0.002 and 0.01 mg kg -1 , and satisfactory linearity with correlation coefficients (R > 0.99) for each dye in all samples was achieved. Compared with the Chinese standard method and the published methods, the proposed method was simplified greatly with much lower requirement of sorbent (5.0 mg) and organic solvent (2.8 mL) and higher sample preparation speed (10 min/sample), while higher recovery (83.6-116.5%) and precision (RSDs < 7.1%) were obtained. With this developed method, we have successfully detected illegal ionic dyes in three common representative foods: yellow croaker, soybean products, and chili seasonings. Graphical abstract Schematic representation of the process of the three-step sample preparation.

  4. [[Chiral separation of five arylpropionic acid drugs and determination of their enantiomers in pharmaceutical preparations by reversed-phase high performance liquid chromatography with cellulose-tris-(4-methylbenzoate) stationary phase

    Science.gov (United States)

    Luo, An; Wan, Qiang; Fan, Huajun; Chen, Zhi; Wu, Xuehao; Huang, Xiaowen; Zang, Linquan

    2014-09-01

    Chromatographic behaviors for enantiomeric separation of arylpropionic acid drugs were systematically developed by reversed phase-high performance liquid chromatography (RP-HPLC) using cellulose-tris-(4-methylbenzoate) (CTMB) as chiral stationary phase (CSP). The effects of the composition of the mobile phase, additives and temperature on chiral separation of flurbiprofen, pranoprofen, naproxen, ibuprofen and loxoprofen were further investigated. The enantiomers had been successfully separated on CSP of CTMB by the mobile phase of methanol-0.1% (v/v) formic acid except naproxen by acetonitrile-0.1% (v/v) formic acid at 25 °C. The mechanisms of the racemic resolution for the above mentioned five drugs are discussed thermodynamically and structurally. The resolutions between respective enantiomers for arylpropionic acid drugs on CTMB had significant differences due to their chromatographic behaviors. The order of resolutions ranked pranoprofen, loxoprofen, flurbiprofen, ibuprofen and naproxen. The method established has been successfully applied to the determination of the enantiomers of the five drugs in commercial preparations under the optimized conditions. It proved that the method is simple, reliable and accurate.

  5. A series of spinel phase cathode materials prepared by a simple hydrothermal process for rechargeable lithium batteries

    Science.gov (United States)

    Liang, Yan-Yu; Bao, Shu-Juan; Li, Hu-Lin

    2006-07-01

    A series of spinel-structured materials have been prepared by a simple hydrothermal procedure in an aqueous medium. The new synthetic method is time and energy saving i.e., no further thermal treatment and extended grinding. The main experimental process involved the insertion of lithium into electrolytic manganese dioxide with glucose as a mild reductant in an autoclave. Both the hydrothermal temperature and the presence of glucose play the critical roles in determining the final spinel integrity. Particular electrochemical performance has also been systematically explored, and the results show that Al 3+, F - co-substituted spinels have the best combination of initial capacity and capacity retention among all these samples, exhibited the initial capacity of 115 mAh/g and maintained more than 90% of the initial value at the 50th cycle.

  6. Preparation and characterization of phase-pure anatase and rutile TiO2 powder by new chemistry route

    International Nuclear Information System (INIS)

    Pereira, E. A.; Montanhera, M.A.; Paula, F.R.; Spada, E.R.

    2014-01-01

    Titanium dioxide (TiO 2 ) is used in a wire range applications such as photocatalysis and sensor device. In this work is shown a new and effective method for the preparation of TiO 2 nanocrystalline in the crystallographic forms, anatase and rutile. The method involves dissolving the TiOSO 4 powder in H 2 O 2 solution and thermal treatment of amorphous precipitate. The technique of X-ray diffraction was used to follow the structure evolution of amorphous precipitate. Pure anatase structure and rutile are obtained at 600 deg C and 1000 deg C with a grain size estimated 24 and 55 nm respectively. TiO 2 nanoparticles is a promising alternative of the low cost whose potential for solar cells deserve a careful evaluation, especially in hybrid solar cells that employs TiO 2 as electron acceptor and as transport channels. (author)

  7. Preparation and thermal properties of form-stable palmitic acid/active aluminum oxide composites as phase change materials for latent heat storage

    International Nuclear Information System (INIS)

    Fang, Guiyin; Li, Hui; Cao, Lei; Shan, Feng

    2012-01-01

    Form-stable palmitic acid (PA)/active aluminum oxide composites as phase change materials were prepared by adsorbing liquid palmitic acid into active aluminum oxide. In the composites, the palmitic acid was used as latent heat storage materials, and the active aluminum oxide was used as supporting material. Fourier transformation infrared spectroscope (FT-IR), X-ray diffractometer (XRD) and scanning electronic microscope (SEM) were used to determine the chemical structure, crystalloid phase and microstructure of the composites, respectively. The thermal properties and thermal stability were investigated by a differential scanning calorimeter (DSC) and a thermogravimetry analyzer (TGA). The FT-IR analyses results indicated that there is no chemical interaction between the palmitic acid and active aluminum oxide. The SEM results showed that the palmitic acid was well adsorbed into porous network of the active aluminum oxide. The DSC results indicated that the composites melt at 60.25 °C with a latent heat of 84.48 kJ kg −1 and solidify at 56.86 °C with a latent heat of 78.79 kJ kg −1 when the mass ratio of the PA to active aluminum oxide is 0.9:1. Compared with that of the PA, the melting and solidifying time of the composites CPCM5 was reduced by 20.6% and 21.4% because of the increased heat transfer rate through EG addition. The TGA results showed that the active aluminum oxide can improve the thermal stability of the composites. -- Highlights: ► Form-stable PA/active aluminum oxide composites as PCMs were prepared. ► Chemical structure, crystalloid phase and microstructure of composites were determined. ► Thermal properties and thermal stability of the composites were investigated. ► Expanded graphite can improve thermal conductivity of the composites.

  8. Effect of preparation conditions on fractal structure and phase transformations in the synthesis of nanoscale M-type barium hexaferrite

    Energy Technology Data Exchange (ETDEWEB)

    Pashkova, E.V. [V.I. Vernadskii Institute of General and Inorganic Chemistry, 32/34 Prospect Palladina, Kyiv-142, 03680 (Ukraine); Solovyova, E.D., E-mail: solovyovak@mail.ru [V.I. Vernadskii Institute of General and Inorganic Chemistry, 32/34 Prospect Palladina, Kyiv-142, 03680 (Ukraine); Kotenko, I.E., E-mail: Hab2420@yahoo.com [National Technical University of Ukraine ' KPI' , Pr. Pobedy, 37, Kyiv-57 (Ukraine); Kolodiazhnyi, T.V., E-mail: kolodiazhnyi.taras@nims.go.jp [National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Belous, A.G., E-mail: belous@ionc.kar.net [V.I. Vernadskii Institute of General and Inorganic Chemistry, 32/34 Prospect Palladina, Kyiv-142, 03680 (Ukraine)

    2011-10-15

    The conditions of the synthesis of carbonate-hydroxide precursors (pH of FeOOH precipitation and heat treatment regimes) were studied in terms of their effect on the fractal structure and physical-chemical properties of precursors. Phase transformations which occur during the synthesis of nanosize M-type barium hexaferrite (BHF) were studied as well. The first structural level of precursors' aggregation for mass fractals, the correlation between fractal dimension and precursors' activity during the synthesis of BHF were determined. Synthesis parameters for the precursors with the optimal fractal structure were determined. These data permit an enhancement of the filtration coefficient of the precipitates by a factor of 4-5, obtaining substantial decrease in the temperature required for synthesis of a single-phase BHF, and monodispersed plate-like nanoparticles (60 nm diameter) with the shape anisotropy and good magnetic characteristics (saturation magnetization (M{sub s})=68,7 emu/g and coercitivity (H{sub c})=5440 Oe). - Highlights: > The nanosize M-type BHF obtained by precipitation of hydroxicarbonates technique. > Optimal fractal structure of a precursor for nanosize M-type BHF has been determined. > The precursor precipitated at pH 4.3 allows getting monodisperse particles of BHF.

  9. Opinions of forest administration chief officers in Artvin Regional Directorate of Forestry about preparation and application phases of forest management plans

    Directory of Open Access Journals (Sweden)

    Rahmi Yılma

    2016-10-01

    Full Text Available In this study, based on the example of Artvin Regional Directorate of Forestry, it is aimed to display the viewpoints of forest administration chief officers as regards planning who are the basic elements of interest groups and who implement plans, determine their opinions about the problems they encounter during preparation and application phases of plans, and develop solution proposals. Within this study a survey was performed with 31 forest administration chief officers in Artvin Regional Directorate of Forestry. According to the survey results, at planning phase it has been seen that participatory processes are put into force, certain criteria and indicators are adopted in differentiating between forest functions at inventory stage, which were also taken into consideration during planning, and in particularly stand parameters were determined accurately. Also during planning phase, it is believed that, endemic, rare and endangered targeted plant and wild animal species are evaluated, whereas non-wood forest types suffer from a lack of evaluation. In addition, it was concluded that lack or insufficiency of silviculture plans, the size of forest administration chiefdom and relations problems between forest administration and local people were being experienced. By integrating other interest groups to planning process, widening the scope of the sudty and realizing similar studies in different regional directorates of forestry, we can determine common points and differences and by this way new strategies can be developed.

  10. Investigation of phase stability of novel equiatomic FeCoNiCuZn based-high entropy alloy prepared by mechanical alloying

    Science.gov (United States)

    Soni, Vinay Kumar; Sanyal, S.; Sinha, S. K.

    2018-05-01

    The present work reports the structural and phase stability analysis of equiatomic FeCoNiCuZn High entropy alloy (HEA) systems prepared by mechanical alloying (MA) method. In this research effort some 1287 alloy combinations were extensively studied to arrive at most favourable combination. FeCoNiCuZn based alloy system was selected on the basis of physiochemical parameters such as enthalpy of mixing (ΔHmix), entropy of mixing (ΔSmix), atomic size difference (ΔX) and valence electron concentration (VEC) such that it fulfils the formation criteria of stable multi component high entropy alloy system. In this context, we have investigated the effect of novel alloying addition in view of microstructure and phase formation aspect. XRD plots of the MA samples shows the formation of stable solid solution with FCC (Face Cantered Cubic) after 20 hr of milling time and no indication of any amorphous or intermetallic phase formation. Our results are in good agreement with calculation and analysis done on the basis of physiochemical parameters during selection of constituent elements of HEA.

  11. [Preparation of Coated CMC-Fe0 Using Rheological Phase Reaction Method and Research on Degradation of TCE in Water].

    Science.gov (United States)

    Fan, Wen-jing; Cheng, Yue; Yu, Shu-zhen; Fan, Xiao-feng

    2015-06-01

    The coated nanoscale zero-valent iron (coated CMC-Fe0) was synthesized with cheap and environment friendly CMC as the coating agent using rheological phase reaction. The sample was characterized by means of XRD, SEM, TEM and N2 adsorption-stripping and used to study reductive dechlorination of TCE. The experimental results indicated that the removal rate of TCE was about 100% when the CMC-Fe0 dosage was 6 g x L(-1), the initial TCE concentration was 5 mg x L(-1) and the reaction time was 40 h. The TCE degradation reaction of coated CMC-Fe0 followed a pseudo-first-order kinetic model. Finally, the product could be simply recovered.

  12. Novel Shape-Stabilized Phase Change Materials Composed of Polyethylene Glycol/Nonsurfactant-Templated Mesoporous Silica: Preparation and Thermal Properties

    Science.gov (United States)

    Chen, Yan; Zhu, Yingying; Wang, Jinbao; Lv, Mengjiao; Zhang, Xiongjie; Gao, Junkai; Zhang, Zijun; Lei, Hao

    2017-12-01

    A novel shape-stabilized phase change material (PEG/TAMS), fabricated using tannic acid-templated mesoporous silica (TAMS) as a support for polyethylene glycol, was developed for thermal energy storage. The method used to synthesize TAMS was simple, cost effective, environmentally friendly, and free of surfactant. The characterization results indicated that PEG was physically absorbed to TAMS and that TAMS had no influence on the crystal structure of PEG. According to the TGA thermograms, PEG/TAMS has excellent thermal stability and can be applied over a wide temperature range. Additionally, the differential scanning calorimetry results suggested that PEG/TAMS has good thermal properties and that its fusion and solidification enthalpies reached 114.7 J/g and 102.4 J/g, respectively. The results indicated that PEG/TAMS has great potential for practical applications.

  13. Preparation of mesoporous nanofibers by vapor phase synthesis: control of mesopore structures with the aid of co-surfactants

    International Nuclear Information System (INIS)

    Min, Sa Hoon; Jang, Jyongsik; Lee, Kyung Jin; Bae, Joonwon

    2013-01-01

    Mesoporous nanofibers (MSNFs) can be fabricated in the pores of anodic aluminum oxide (AAO) membrane using diverse methods. Among them vapor phase synthesis (VPS) provides several advantages over sol–gel or evaporation-induced self-assembly (EISA) based methods. One powerful advantage is that we can employ multiple surfactants as structural directing agents (SDAs) simultaneously. By adopting diverse pairs of SDAs, we can control the mesopore structures, i.e. pore size, surface area, and even the morphology of mesostructures. Here, we used F127 as a main SDA, which is relatively robust (thus, difficult to change the mesopore structures), and added a series of cationic co-surfactants to observe the systematical changes in their mesostructure with respect to the chain length of the co-surfactant. (paper)

  14. Preparation of mesoporous nanofibers by vapor phase synthesis: control of mesopore structures with the aid of co-surfactants

    Energy Technology Data Exchange (ETDEWEB)

    Min, Sa Hoon; Jang, Jyongsik; Lee, Kyung Jin [School of Chemical and Biological Engineering, College of Engineering, Seoul National University, Shinlimdong 56-1, Seoul, 151-742 (Korea, Republic of); Bae, Joonwon [Department of Applied Chemistry, Dongduk Women' s University, Seoul 136-714 (Korea, Republic of)

    2013-06-28

    Mesoporous nanofibers (MSNFs) can be fabricated in the pores of anodic aluminum oxide (AAO) membrane using diverse methods. Among them vapor phase synthesis (VPS) provides several advantages over sol-gel or evaporation-induced self-assembly (EISA) based methods. One powerful advantage is that we can employ multiple surfactants as structural directing agents (SDAs) simultaneously. By adopting diverse pairs of SDAs, we can control the mesopore structures, i.e. pore size, surface area, and even the morphology of mesostructures. Here, we used F127 as a main SDA, which is relatively robust (thus, difficult to change the mesopore structures), and added a series of cationic co-surfactants to observe the systematical changes in their mesostructure with respect to the chain length of the co-surfactant. (paper)

  15. Preparation of mesoporous nanofibers by vapor phase synthesis: control of mesopore structures with the aid of co-surfactants

    Science.gov (United States)

    Min, Sa Hoon; Bae, Joonwon; Jang, Jyongsik; Lee, Kyung Jin

    2013-06-01

    Mesoporous nanofibers (MSNFs) can be fabricated in the pores of anodic aluminum oxide (AAO) membrane using diverse methods. Among them vapor phase synthesis (VPS) provides several advantages over sol-gel or evaporation-induced self-assembly (EISA) based methods. One powerful advantage is that we can employ multiple surfactants as structural directing agents (SDAs) simultaneously. By adopting diverse pairs of SDAs, we can control the mesopore structures, i.e. pore size, surface area, and even the morphology of mesostructures. Here, we used F127 as a main SDA, which is relatively robust (thus, difficult to change the mesopore structures), and added a series of cationic co-surfactants to observe the systematical changes in their mesostructure with respect to the chain length of the co-surfactant.

  16. Preparation of 2-in.-diameter (001) β-Ga2O3 homoepitaxial wafers by halide vapor phase epitaxy

    Science.gov (United States)

    Thieu, Quang Tu; Wakimoto, Daiki; Koishikawa, Yuki; Sasaki, Kohei; Goto, Ken; Konishi, Keita; Murakami, Hisashi; Kuramata, Akito; Kumagai, Yoshinao; Yamakoshi, Shigenobu

    2017-11-01

    The homoepitaxial growth of thick β-Ga2O3 layers on 2-in.-diameter (001) wafers was demonstrated by halide vapor phase epitaxy. Growth rates of 3 to 4 µm/h were confirmed for growing intentionally Si-doped n-type layers. A homoepitaxial layer with an average thickness and carrier concentration of 10.9 µm and 2.7 × 1016 cm-3 showed standard deviations of 1.8 µm (16.5%) and 0.5 × 1016 cm-3 (19.7%), respectively. Ni Schottky barrier diodes fabricated directly on a 5.3-µm-thick homoepitaxial layer with a carrier concentration of 3.4 × 1016 cm-3 showed reasonable reverse and forward characteristics, i.e., breakdown voltages above 200 V and on-resistances of 3.8-7.7 mΩ cm2 at room temperature.

  17. Preparation and enhanced oxidation performance of a Hf-doped single-phase Pt-modified aluminide coating

    International Nuclear Information System (INIS)

    Yang, Y.F.; Jiang, C.Y.; Yao, H.R.; Bao, Z.B.; Zhu, S.L.; Wang, F.H.

    2016-01-01

    Graphical abstract: Tiny Hf particles were successfully incorporated into Pt plating via simple electro-plating method. The hafnium particles were either nipped at Pt grain boundaries or wrapped inside Pt grains, and most of them were below 3 μm in size, showing a uniform distribution within the Pt plating. - Highlights: • A Hf-rich belt formed between outer (Ni,Pt)Al and IDZ after aluminisation. • Hf-doped coating showed much decreased mass gain and oxidation rate constant k_p. • Hf-rich belt acted as diffusion barrier by restraining diffusions of Al and W. • Degradation of β was effectively postponed by the unique Hf addition. • Hf-doped coating exhibited lighter oxide scale rumpling tendency. - Abstract: A Hf-doped β-(Ni,Pt)Al coating was prepared by co-deposition of a Pt-Hf composite plating and successive aluminisation. Then, a distinct Hf-rich belt was formed internally between the outer additive (Ni,Pt)Al coating and interdiffusion zone. An isothermal oxidation test at 1100 °C revealed a relatively lower oxidation rate constant and decreased oxide scale rumpling tendency for the Hf-doped coating during which the Hf-rich belt partly acted as an effective diffusion barrier. The unique addition of Hf into a β-(Ni,Pt)Al coating can delay the transitional oxidation period from transient alumina to stable one and postpone the degradation from β to γ'.

  18. Preparation and evaluation of a novel molecularly imprinted polymer coating for selective extraction of indomethacin from biological samples by electrochemically controlled in-tube solid phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Asiabi, Hamid [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Seidi, Shahram; Ghahramanifard, Fazel [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of)

    2016-03-24

    In the present work, an automated on-line electrochemically controlled in-tube solid-phase microextraction (EC-in-tube SPME) coupled with HPLC-UV was developed for the selective extraction and preconcentration of indomethacin as a model analyte in biological samples. Applying an electrical potential can improve the extraction efficiency and provide more convenient manipulation of different properties of the extraction system including selectivity, clean-up, rate, and efficiency. For more enhancement of the selectivity and applicability of this method, a novel molecularly imprinted polymer coated tube was prepared and applied for extraction of indomethacin. For this purpose, nanostructured copolymer coating consisting of polypyrrole doped with ethylene glycol dimethacrylate was prepared on the inner surface of a stainless-steel tube by electrochemical synthesis. The characteristics and application of the tubes were investigated. Electron microscopy provided a cross linked porous surface and the average thickness of the MIP coating was 45 μm. Compared with the non-imprinted polymer coated tubes, the special selectivity for indomethacin was discovered with the molecularly imprinted coated tube. Moreover, stable and reproducible responses were obtained without being considerably influenced by interferences commonly existing in biological samples. Under the optimal conditions, the limits of detection were in the range of 0.07–2.0 μg L{sup −1} in different matrices. This method showed good linearity for indomethacin in the range of 0.1–200 μg L{sup −1}, with coefficients of determination better than 0.996. The inter- and intra-assay precisions (RSD%, n = 3) were respectively in the range of 3.5–8.4% and 2.3–7.6% at three concentration levels of 7, 70 and 150 μg L{sup −1}. The results showed that the proposed method can be successfully applied for selective analysis of indomethacin in biological samples. - Graphical abstract: An automated on

  19. Solid-phase extraction combined with dispersive liquid-liquid microextraction and chiral liquid chromatography-tandem mass spectrometry for the simultaneous enantioselective determination of representative proton-pump inhibitors in water samples.

    Science.gov (United States)

    Zhao, Pengfei; Deng, Miaoduo; Huang, Peiting; Yu, Jia; Guo, Xingjie; Zhao, Longshan

    2016-09-01

    This report describes, for the first time, the simultaneous enantioselective determination of proton-pump inhibitors (PPIs-omeprazole, lansoprazole, pantoprazole, and rabeprazole) in environmental water matrices based on solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME) and chiral liquid chromatography-tandem mass spectrometry. The optimized results of SPE-DLLME were obtained with PEP-2 column using methanol-acetonitrile (1/1, v/v) as elution solvent, dichloroethane, and acetonitrile as extractant and disperser solvent, respectively. The separation and determination were performed using reversed-phase chromatography on a cellulose chiral stationary phase, a Chiralpak IC (250 mm × 4.6 mm, 5 μm) column, under isocratic conditions at 0.6 mL min(-1) flow rate. The analytes were detected in multiple reaction monitoring (MRM) mode by triple quadrupole mass spectrometry. Isotopically labeled internal standards were used to compensate matrix interferences. The method provided enrichment factors of around 500. Under optimal conditions, the mean recoveries for all eight enantiomers from the water samples were 89.3-107.3 % with 0.9-10.3 % intra-day RSD and 2.3-8.1 % inter-day RSD at 20 and 100 ng L(-1) levels. Correlation coefficients (r (2)) ≥ 0.999 were achieved for all enantiomers within the range of 2-500 μg L(-1). The method detection and quantification limits were at very low levels, within the range of 0.67-2.29 ng L(-1) and 2.54-8.68 ng L(-1), respectively. This method was successfully applied to the determination of the concentrations and enantiomeric fractions of the targeted analytes in wastewater and river water, making it applicable to the assessment of the enantiomeric fate of PPIs in the environment. Graphical Abstract Simultaneous enantioselective determination of representative proton-pump inhibitors in water samples.

  20. Microextraction by Packed Sorbent (MEPS and Solid-Phase Microextraction (SPME as Sample Preparation Procedures for the Metabolomic Profiling of Urine

    Directory of Open Access Journals (Sweden)

    Catarina Silva

    2014-01-01

    Full Text Available For a long time, sample preparation was unrecognized as a critical issue in the analytical methodology, thus limiting the performance that could be achieved. However, the improvement of microextraction techniques, particularly microextraction by packed sorbent (MEPS and solid-phase microextraction (SPME, completely modified this scenario by introducing unprecedented control over this process. Urine is a biological fluid that is very interesting for metabolomics studies, allowing human health and disease characterization in a minimally invasive form. In this manuscript, we will critically review the most relevant and promising works in this field, highlighting how the metabolomic profiling of urine can be an extremely valuable tool for the early diagnosis of highly prevalent diseases, such as cardiovascular, oncologic and neurodegenerative ones.

  1. Triterpene-loaded microemulsion using Coix lacryma-jobi seed extract as oil phase for enhanced antitumor efficacy: preparation and in vivo evaluation

    Directory of Open Access Journals (Sweden)

    Qu D

    2013-12-01

    Full Text Available Ding Qu, Junjie He, Congyan Liu, Jing Zhou, Yan ChenKey Laboratory of New Drug Delivery System of Chinese Materia Medica, Jiangsu Provincial Academy of Chinese Medicine, Jiangsu, People’s Republic of ChinaAbstract: Ganoderma lucidum triterpene-loaded microemulsions (TMEs using Coix lacryma-jobi (adlay seed oil as oil phase were prepared, characterized, and evaluated for enhanced antitumor activity. Ternary phase diagrams for the TMEs were constructed and the optimal preparation was developed. Transmission electron microscopy and dynamic light scattering showed that this formulation had a well defined spherical shape, a homogeneous distribution, a small size, and a narrow polydispersity index. The drug-loading rate was determined to be 9.87% by ultraviolet spectrophotometry, and acceptable stability under various stimulations in vitro was confirmed. Importantly, the TME formulation showed a significantly greater antiproliferative effect towards human lung carcinoma (A549 cells and murine lung tumor (Lewis cells in comparison with suspension formulations containing triterpene and adlay seed oil as a positive control. The half-maximal inhibitory concentration of the TMEs was about 0.62 mg crude drug per mL, being 2.5-fold improved relative to that of the corresponding suspension formulation, but no significant cytotoxicity was observed for the bare microemulsion in A549 cells and Lewis cells. In vivo, the TME formulation showed markedly enhanced antitumor efficacy in a xenograft model of Lewis lung cancer after intragastric administration. Compared with cyclophosphamide, the TME formulation showed similar antitumor activity but less general toxicity. These results indicate the feasibility of using a microemulsion to increase the solubility of triterpene and adlay. TMEs hold promise as an efficient drug delivery system for the treatment of lung cancer.Keywords: microemulsion, Ganoderma lucidum, triterpene, adlay seed oil, lung cancer

  2. Large-volume injection of sample diluents not miscible with the mobile phase as an alternative approach in sample preparation for bioanalysis: an application for fenspiride bioequivalence.

    Science.gov (United States)

    Medvedovici, Andrei; Udrescu, Stefan; Albu, Florin; Tache, Florentin; David, Victor

    2011-09-01

    Liquid-liquid extraction of target compounds from biological matrices followed by the injection of a large volume from the organic layer into the chromatographic column operated under reversed-phase (RP) conditions would successfully combine the selectivity and the straightforward character of the procedure in order to enhance sensitivity, compared with the usual approach of involving solvent evaporation and residue re-dissolution. Large-volume injection of samples in diluents that are not miscible with the mobile phase was recently introduced in chromatographic practice. The risk of random errors produced during the manipulation of samples is also substantially reduced. A bioanalytical method designed for the bioequivalence of fenspiride containing pharmaceutical formulations was based on a sample preparation procedure involving extraction of the target analyte and the internal standard (trimetazidine) from alkalinized plasma samples in 1-octanol. A volume of 75 µl from the octanol layer was directly injected on a Zorbax SB C18 Rapid Resolution, 50 mm length × 4.6 mm internal diameter × 1.8 µm particle size column, with the RP separation being carried out under gradient elution conditions. Detection was made through positive ESI and MS/MS. Aspects related to method development and validation are discussed. The bioanalytical method was successfully applied to assess bioequivalence of a modified release pharmaceutical formulation containing 80 mg fenspiride hydrochloride during two different studies carried out as single-dose administration under fasting and fed conditions (four arms), and multiple doses administration, respectively. The quality attributes assigned to the bioanalytical method, as resulting from its application to the bioequivalence studies, are highlighted and fully demonstrate that sample preparation based on large-volume injection of immiscible diluents has an increased potential for application in bioanalysis.

  3. Liquid-phase sample preparation method for real-time monitoring of airborne asbestos fibers by dual-mode high-throughput microscopy.

    Science.gov (United States)

    Cho, Myoung-Ock; Kim, Jung Kyung; Han, Hwataik; Lee, Jeonghoon

    2013-01-01

    Asbestos that had been used widely as a construction material is a first-level carcinogen recognized by the World Health Organization. It can be accumulated in body by inhalation causing virulent respiratory diseases including lung cancer. In our previous study, we developed a high-throughput microscopy (HTM) system that can minimize human intervention accompanied by the conventional phase contrast microscopy (PCM) through automated counting of fibrous materials and thus significantly reduce analysis time and labor. Also, we attempted selective detection of chrysotile using DksA protein extracted from Escherichia coli through a recombinant protein production technique, and developed a dual-mode HTM (DM-HTM) by upgrading the HTM device. We demonstrated that fluorescently-labeled chrysotile asbestos fibers can be identified and enumerated automatically among other types of asbestos fibers or non-asbestos particles in a high-throughput manner through a newly modified HTM system for both reflection and fluorescence imaging. However there is a limitation to apply DM-HTM to airborne sample with current air collecting method due to the difficulty of applying the protein to dried asbestos sample. Here, we developed a technique for preparing liquid-phase asbestos sample using an impinger normally used to collect odor molecules in the air. It would be possible to improve the feasibility of the dual-mode HTM by integrating a sample preparation unit for making collected asbestos sample dispersed in a solution. The new technique developed for highly sensitive and automated asbestos detection can be a potential alternative to the conventional manual counting method, and it may be applied on site as a fast and reliable environmental monitoring tool.

  4. Preparation of lithium indium oxide via a rheological phase route and its electrochemical characteristics in LiOH and Li{sub 2}SO{sub 4} solutions

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Guo-Qing [Department of Chemistry and Environment Science of Yangtze Normal University, 408100 Chongqing (China); College of Chemistry and Chemical Engineering of Chongqing University, Chongqing 400030 (China); Zhang, Sheng-Tao [College of Chemistry and Chemical Engineering of Chongqing University, Chongqing 400030 (China); Wu, Xing-Fa [Department of Chemistry and Environment Science of Yangtze Normal University, 408100 Chongqing (China)

    2010-01-15

    Submicrometer-sized lithium indium oxide (LiInO{sub 2}) powder via a rheological phase method using trilithium citrate tetra hydrate (C{sub 6}H{sub 5}Li{sub 3}O{sub 7} . 4H{sub 2}O) and indium oxide (In{sub 2}O{sub 3}) has been prepared in this work for the first time. The optimal pyrolyzing temperature range to prepare crystalline LiInO{sub 2} is between 650 and 900 C, which was confirmed by thermal gravimetric and differential thermogravimetric analysis of the precursor and X-ray diffraction analysis. The pure phase LiInO{sub 2} sample obtained has a uniform particle morphology and submicrosize, which was observed by scanning electron microscopy. The electrochemical studies show that a new pair of cathodic and anodic peaks at 0.23 and 0.38 V (vs. saturated calomel electrode) was obviously observed from the cyclic voltammetry curve of LiInO{sub 2} in 1 M LiOH solution, indicating a battery characteristic of the material in this electrolyte. While in 1 M Li{sub 2}SO{sub 4} solution, the sample presents a supercapacitive characteristic within the same potential range. The reasons for different electrochemical behaviors in these two electrolytes can be attributed to the fact that the reaction of lithium ion insertion/extraction into/out of a LiInO{sub 2} electrode takes place in the bulk material in LiOH electrolyte solution, whereas it takes place on the electrode/electrolyte interface for Li{sub 2}SO{sub 4} electrolyte case. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  5. Properties of form-stable paraffin/silicon dioxide/expanded graphite phase change composites prepared by sol–gel method

    International Nuclear Information System (INIS)

    Li, Min; Wu, Zhishen; Tan, Jinmiao

    2012-01-01

    Highlights: ► Paraffin/SiO 2 /EG composite PCM was prepared with sol–gel method. ► The thermal conductivity of SiO 2 /paraffin/EG is 94.7% higher than paraffin. ► The latent heat of paraffin/SiO 2 /EG composite is 104.4 J/g. -- Abstract: A form-stable paraffin/silicon dioxide (SiO 2 )/expanded graphite (EG) composite phase change material (PCM) was prepared by sol–gel method. Silica gel acts as the supporting material and EG is used to increase the thermal conductivity. The mass fractions of silicon oxide and graphite are 20.8% and 7.2%, respectively. The composite PCM was characterized using scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transformation infrared spectroscopy (FTIR) method. Thermal properties and thermal stability of the composite PCM were studied using differential scanning calorimetry (DSC). The result shows that paraffin was well dispersed in the network of silica gel and there is no chemical reaction between them. The phase change temperature of the paraffin/SiO 2 composite and the paraffin/SiO 2 /EG composite are 27.53 °C and 27.72 °C, respectively. The latent heat of the paraffin/SiO 2 composite and the paraffin/SiO 2 /EG composite are 112.8 J/g and 104.4 J/g, respectively. The thermal conductivity of the SiO 2 /paraffin composite and the SiO 2 /paraffin/EG composite are 28.2% and 94.7% higher than that of paraffin.

  6. One-step liquid phase chemical method to prepare carbon-based amorphous molybdenum sulfides: As the effective hydrogen evolution reaction catalysts

    International Nuclear Information System (INIS)

    Guo, Mengmeng; Wu, Qikang; Yu, Miaomiao; Wang, Yinling; Li, Maoguo

    2017-01-01

    Two different kinds of carbon-based amorphous molybdenum sulfide composite catalysts (activated carbon supported amorphous molybdenum sulfide and acetylene black supported amorphous molybdenum sulfide) had been prepared in a facile and scalable one-step liquid phase chemical method. The morphological and structural information of catalysts was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-Ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and it’s electro-catalytic HER activity were evaluated by linear sweep voltammetry(LSV), amperometric i-t technology and AC impedance technology. The as-prepared carbon-based amorphous molybdenum sulfides showed greatly enhanced electro-catalytic activity for HER compared with pure amorphous molybdenum sulfides. Especially, the nano-sized acetylene black supported molybdenum sulfide exhibited excellent electro-catalytic HER performances with a low onset potential of −116 mV versus reverse hydrogen electrode (RHE) and a small Tafel slope of 51 mV per decade.

  7. Preparation and thermal properties of mineral-supported polyethylene glycol as form-stable composite phase change materials (CPCMs) used in asphalt pavements.

    Science.gov (United States)

    Jin, Jiao; Lin, Feipeng; Liu, Ruohua; Xiao, Ting; Zheng, Jianlong; Qian, Guoping; Liu, Hongfu; Wen, Pihua

    2017-12-05

    Three kinds of mineral-supported polyethylene glycol (PEG) as form-stable composite phase change materials (CPCMs) were prepared to choose the most suitable CPCMs in asphalt pavements for the problems of asphalt pavements rutting diseases and urban heat islands. The microstructure and chemical structure of CPCMs were characterized by SEM, FT-IR and XRD. Thermal properties of the CPCMs were determined by TG and DSC. The maximum PEG absorption of diatomite (DI), expanded perlite (EP) and expanded vermiculite (EVM) could reach 72%, 67% and 73.6%, respectively. The melting temperatures and latent heat of CPCMs are in the range of 52-55 °C and 100-115 J/g, respectively. The results show that PEG/EP has the best thermal and chemical stability after 100 times of heating-cooling process. Moreover, crystallization fraction results show that PEG/EP has slightly higher latent heats than that of PEG/DI and PEG/EVM. Temperature-adjusting asphalt mixture was prepared by substituting the fine aggregates with PEG/EP CPCMs. The upper surface maximum temperature difference of temperature-adjusting asphalt mixture reaches about 7.0 °C in laboratory, and the surface peak temperature reduces up to 4.3 °C in the field experiment during a typical summer day, indicating a great potential application for regulating pavement temperature field and alleviating the urban heat islands.

  8. Preparation of sulfonated graphene/polypyrrole solid-phase microextraction coating by in situ electrochemical polymerization for analysis of trace terpenes.

    Science.gov (United States)

    Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

    2014-06-13

    In this study, a novel sulfonated graphene/polypyrrole (SG/PPy) solid-phase microextraction (SPME) coating was prepared and fabricated on a stainless-steel wire by a one-step in situ electrochemical polymerization method. Crucial preparation conditions were optimized as polymerization time of 15min and SG doping amount of 1.5mg/mL. SG/PPy coating showed excellent thermal stability and mechanical durability with a long lifespan of more than 200 stable replicate extractions. SG/PPy coating demonstrated higher extraction selectivity and capacity to volatile terpenes than commonly-used commercial coatings. Finally, SG/PPy coating was practically applied for the analysis of volatile components from star anise and fennel samples. The majority of volatile components identified were terpenes, which suggested the ultra-high extraction selectivity of SG/PPy coating to terpenes during real analytical projects. Four typical volatile terpenes were further quantified to be 0.2-27.4μg/g from star anise samples with good recoveries of 76.4-97.8% and 0.1-1.6μg/g from fennel samples with good recoveries of 80.0-93.1%, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Green Preparation of Epoxy/Graphene Oxide Nanocomposites Using a Glycidylamine Epoxy Resin as the Surface Modifier and Phase Transfer Agent of Graphene Oxide.

    Science.gov (United States)

    Tang, Xinlei; Zhou, Yang; Peng, Mao

    2016-01-27

    In studies of epoxy/graphene oxide (GO) nanocomposites, organic solvents are commonly used to disperse GO, and vigorous mechanical processes and complicated modification of GO are usually required, increasing the cost and hindering the development and application of epoxy nanocomposites. Here, we report a green, facile, and efficient method of preparing epoxy/GO nanocomposites. When triglycidyl para-aminophenol (TGPAP), a commercially available glycidyl amine epoxy resin with one tertiary amine group per molecule, is used as both the surface modifier and phase transfer agent of GO, GO can be directly and rapidly transferred from water to diglycidyl ether of bisphenol A and other types of epoxy resins by manual stirring under ambient conditions, whereas GO cannot be transferred to these epoxy resins in the absence of TGPAP. The interaction between TGPAP and GO and the effect of the TGPAP content on the dispersion of GO in the epoxy matrix were investigated systematically. Superior dispersion and exfoliation of GO nanosheets and remarkably improved mechanical properties, including tensile and flexural properties, toughness, storage modulus, and microhardness, of the epoxy/GO nanocomposites with a suitable amount of TGPAP were demonstrated. This method is organic-solvent-free and technically feasible for large-scale preparation of high-performance nanocomposites; it opens up new opportunities for exploiting the unique properties of graphene or even other nanofillers for a wide range of applications.

  10. Preparation, characterization and thermal properties of styrene maleic anhydride copolymer (SMA)/fatty acid composites as form stable phase change materials

    International Nuclear Information System (INIS)

    Sari, Ahmet; Alkan, Cemil; Karaipekli, Ali; Onal, Adem

    2008-01-01

    Fatty acids such as stearic acid (SA), palmitic acid (PA), myristic acid (MA) and lauric acid (LA) are promising phase change materials (PCMs) for latent heat thermal energy storage (LHTES) applications, but high cost is the major drawback of them, limiting their utility area in thermal energy storage. The use of fatty acids as form stable PCMs will increase their feasibilities in practical applications due to the reduced cost of the LHTES system. In this regard, a series of styrene maleic anhydride copolymer (SMA)/fatty acid composites, SMA/SA, SMA/PA, SMA/MA, and SMA/LA, were prepared as form stable PCMs by encapsulation of fatty acids into the SMA, which acts as a supporting material. The encapsulation ratio of fatty acids was as much as 85 wt.% and no leakage of fatty acid was observed even when the temperature of the form stable PCM was over the melting point of the fatty acid in the composite. The prepared form stable composite PCMs were characterized using optic microscopy (OM), viscosimetry and Fourier transform infrared (FT-IR) spectroscopy methods, and the results showed that the SMA was physically and chemically compatible with the fatty acids. In addition, the thermal characteristics such as melting and freezing temperatures and latent heats of the form stable composite PCMs were measured by using the differential scanning calorimetry (DSC) technique, which indicated they had good thermal properties. On the basis of all the results, it was concluded that form stable SMA/fatty acid composite PCMs had important potential for practical LHTES applications such as under floor space heating of buildings and passive solar space heating of buildings by using wallboard, plasterboard or floors impregnated with a form stable PCM due to their satisfying thermal properties, easy preparation in desired dimensions, direct usability without needing additional encapsulation thereby eliminating the thermal resistance caused by the shell and, thus, reducing the cost of

  11. Preparation and properties of 1-tetradecanol/1,3:2,4-di-(3,4-dimethyl) benzylidene sorbitol gelatinous form-stable phase change materials

    International Nuclear Information System (INIS)

    Tian, Tuo; Song, Jian; Niu, Libo; Feng, Rongxiu

    2013-01-01

    Graphical abstract: The 1,3:2,4-di-(3,4-dimethyl) benzylidene sorbitol can self-assemble to form three-dimensional network and immobilized the 1-tetradecanol. As a result, the gel-to-sol transition temperature of the composite PCM increased and the 1-tetradecanol leakage decreased. Highlights: ► First used of 1,3:2,4-di-(3,4-dimethyl) benzylidene sorbitol in alcohol-based PCMs. ► A new method of doping with exfoliated graphite is presented. ► A possible mechanism for decreasing leakage has been proposed based on SEM results. ► The prepared composite PCMs showed a high-energy storage density. ► The addition of exfoliated graphite enhanced the thermal conductivity of the PCMs. - Abstract: A 1-tetradecanol (TD)/1,3:2,4-di-(3,4-dimethyl) benzylidene sorbitol (DMDBS) composite was prepared as a novel form-stable phase change material (PCM), and the properties of the composites such as the gel-to-sol transition temperature, the latent heat, the microstructure and the thermal storage performance were characterized. The composite was prepared by impregnating DMDBS into TD and the maximum feasible weight percentage of TD was determined to be 94.2 wt%. The gel-to-sol transition temperature of the composite PCM was 158.3–180.0 °C, which is well above the melting point of 1-tetradecanol. Differential scanning calorimeter (DSC) was used to determine the melting and freezing enthalpies of 1-tetradecanol in the composite PCM and the values are 218.5 and 215.3 J g −1 , respectively. Scanning electron microscopy (SEM) results showed that 1-tetradecanol dispersed in the three-dimensional network formed by DMDBS. The relationship between the amount of DMDBS additive and the leakage was also discussed. The thermal conductivity of the composite PCM was improved by doping with exfoliated graphite

  12. Preparation of Curcumin-Piperazine Coamorphous Phase and Fluorescence Spectroscopic and Density Functional Theory Simulation Studies on the Interaction with Bovine Serum Albumin.

    Science.gov (United States)

    Pang, Wenzhe; Lv, Jie; Du, Shuang; Wang, Jiaojiao; Wang, Jing; Zeng, Yanli

    2017-09-05

    In the present study, a new coamorphous phase (CAP) of bioactive herbal ingredient curcumin (CUR) with high solubilitythe was screened with pharmaceutically acceptable coformers. Besides, to provide basic information for the best practice of physiological and pharmaceutical preparations of CUR-based CAP, the interaction between CUR-based CAP and bovine serum albumin (BSA) was studied at the molecular level in this paper. CAP of CUR and piperazine with molar ratio of 1:2 was prepared by EtOH-assisted grinding. The as-prepared CAP was characterized by powder X-ray diffraction, modulated temperature differential scanning calorimetry, thermogravimetric analysis, Fourier-transform infrared, and solid-state 13 C nuclear magnetic resonance. The 1:2 CAP stoichioimetry was sustained by C═O···H hydrogen bonds between the N-H group of the piperazine and the C═O group of CUR; piperazine stabilized the diketo structure of CUR in CAP. The dissolution rate of CUR-piperazine CAP in 30% ethanol-water was faster than that of CUR; the t 50 values were 243.1 min for CUR and 4.378 min for CAP. Furthermore, interactions of CUR and CUR-piperazine CAP with BSA were investigated by fluorescence spectroscopy and density functional theory (DFT) calculation. The binding constants (K b ) of CUR and CUR-piperazine CAP with BSA were 10.0 and 9.1 × 10 3 L mol -1 at 298 K, respectively. Moreover, DFT simulation indicated that the interaction energy values of hydrogen-bonded interaction in the tryptophan-CUR and tryptophan-CUR-piperazine complex were -26.1 and -17.9 kJ mol -1 , respectively. In a conclusion, after formation of CUR-piperazine CAP, the interaction forces between CUR and BSA became weaker.

  13. Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

    International Nuclear Information System (INIS)

    He Juan; Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng

    2010-01-01

    A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L -1 . The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

  14. Form-Stable Phase Change Materials Based on Eutectic Mixture of Tetradecanol and Fatty Acids for Building Energy Storage: Preparation and Performance Analysis

    Directory of Open Access Journals (Sweden)

    Yiran li

    2013-10-01

    Full Text Available This paper is focused on preparation and performance analysis of a series of form-stable phase change materials (FSPCMs, based on eutectic mixtures as phase change materials (PCMs for thermal energy storage and high-density polyethylene (HDPE-ethylene-vinyl acetate (EVA polymer as supporting materials. The PCMs were eutectic mixtures of tetradecanol (TD–capric acid (CA, TD–lauric acid (LA, and TD–myristic acid (MA, which were rarely explored before. Thermal properties of eutectic mixtures and FSPCMs were measured by differential scanning calorimeter (DSC. The onset melting/solidification temperatures of form-stable PCMs were 19.13 °C/13.32 °C (FS TD–CA PCM, 24.53 °C/24.92 °C (FS TD–LA PCM, and 33.15 °C/30.72 °C (FS TD–MA PCM, respectively, and latent heats were almost greater than 90 J/g. The surface morphologies and chemical stability of form-stable PCM were surveyed by scanning electron microscopy (SEM and Fourier-transform infrared (FT-IR spectroscopy, respectively. The thermal cycling test revealed that the thermal reliability of these three form-stable PCMs was good. Thermal storage/release experiment indicated melting/solidification time was shortened by introducing 10 wt % aluminum powder (AP. It is concluded that these FSPCMs can act as potential building thermal storage materials in terms of their satisfactory thermal properties.

  15. Preparation, Mechanical and Thermal Properties of Cement Board with Expanded Perlite Based Composite Phase Change Material for Improving Buildings Thermal Behavior

    Directory of Open Access Journals (Sweden)

    Rongda Ye

    2015-11-01

    Full Text Available Here we demonstrate the mechanical properties, thermal conductivity, and thermal energy storage performance of construction elements made of cement and form-stable PCM-Rubitherm® RT 28 HC (RT28/expanded perlite (EP composite phase change materials (PCMs. The composite PCMs were prepared by adsorbing RT28 into the pores of EP, in which the mass fraction of RT28 should be limited to be no more than 40 wt %. The adsorbed RT28 is observed to be uniformly confined into the pores of EP. The phase change temperatures of the RT28/EP composite PCMs are very close to that of the pure RT28. The apparent density and compression strength of the composite cubes increase linearly with the mass fraction of RT28. Compared with the thermal conductivity of the boards composed of cement and EP, the thermal conductivities of the composite boards containing RT28 increase by 15%–35% with the mass fraction increasing of RT28. The cubic test rooms that consist of six boards were built to evaluate the thermal energy storage performance, it is found that the maximum temperature different between the outside surface of the top board with the indoor temperature using the composite boards is 13.3 °C higher than that of the boards containing no RT28. The thermal mass increase of the built environment due to the application of composite boards can contribute to improving the indoor thermal comfort and reducing the energy consumption in the buildings.

  16. Preparation and characterization of magnetic carboxylated nanodiamonds for vortex-assisted magnetic solid-phase extraction of ziram in food and water samples.

    Science.gov (United States)

    Yılmaz, Erkan; Soylak, Mustafa

    2016-09-01

    A simple and rapid vortex-assisted magnetic solid phase extraction (VA-MSPE) method for the separation and preconcentration of ziram (zinc dimethyldithiocarbamate), subsequent detection of the zinc in complex structure of ziram by flame atomic absorption spectrometry (AAS) has been developed. The ziram content was calculated by using stoichiometric relationship between the zinc and ziram. Magnetic carboxylated nanodiamonds (MCNDs) as solid-phase extraction adsorbent was prepared and characterized by Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD) spectrometry and scanning electron microscopy (SEM). These magnetic carboxylated nanodiamonds carrying the ziram could be easily separated from the aqueous solution by applying an external magnetic field; no filtration or centrifugation was necessary. Some important factors influencing the extraction efficiency of ziram such as pH of sample solution, amount of adsorbent, type and volume of eluent, extraction and desorption time and sample volume were studied and optimized. The total extraction and detection time was lower than 10min The preconcentration factor (PF), the precision (RSD, n=7), the limit of detection (LOD) and limit of quantification (LOQ) were 160, 7.0%, 5.3µgL(-1) and 17.5µgL(-1), respectively. The interference of various ions has been examined and the method has been applied for the determination of ziram in various waters, foodstuffs samples and synthetic mixtures. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Solvent-free sample preparation by headspace solid-phase microextraction applied to the tracing of n-butyl nitrite abuse.

    Science.gov (United States)

    Tytgat, J; Daenens, P

    1996-01-01

    The most common alkyl nitrites encountered in forensic toxicology are iso-butyl, n-butyl and iso-pentyl(amyl) nitrites. All have become popular as an aphrodisiac, especially among the homosexual population. Alkyl nitrites are a volatile and unstable group of compounds, which hydrolyse in aqueous matrices to the alcohol and nitrite ion. Here we describe a fast, clean and sensitive procedure for the detection of hydrolysed n-butyl nitrite in whole human blood using a new, solvent-free sampling technique, the headspace solid-phase micro-extraction (HSPME), combined with GC/FID analysis. Sample preparation was investigated using two different stationary phases (100 microns polydimethylsiloxane and 85 microns polyacrylate), coating a fused silica fibre. The effect of different sampling times at fixed temperatures was also studied. Our results demonstrate that the HSPME/GC/FID procedure allows tracing of n-butyl nitrite abuse and detects hydrolysed n-butyl nitrite, i.e., released n-butanol, in whole blood at the 1 ng/mL level.

  18. Preparation and Evaluation of Core–Shell Magnetic Molecularly Imprinted Polymers for Solid-Phase Extraction and Determination of Sterigmatocystin in Food

    Directory of Open Access Journals (Sweden)

    Jing-Min Liu

    2017-10-01

    Full Text Available Magnetic molecularly imprinted polymers (MMIPs, combination of outstanding magnetism with specific selective binding capability for target molecules, have proven to be attractive in separation science and bio-applications. Herein, we proposed the core–shell magnetic molecularly imprinted polymers for food analysis, employing the Fe3O4 particles prepared by co-precipitation protocol as the magnetic core and MMIP film onto the silica layer as the recognition and adsorption of target analytes. The obtained MMIPs materials have been fully characterized by scanning electron microscope (SEM, Fourier transform infrared spectrometer (FT-IR, vibrating sample magnetometer (VSM, and re-binding experiments. Under the optimal conditions, the fabricated Fe3O4@MIPs demonstrated fast adsorption equilibrium, a highly improved imprinting capacity, and excellent specificity to target sterigmatocystin (ST, which have been successfully applied as highly efficient solid-phase extraction materials followed by high-performance liquid chromatography (HPLC analysis. The MMIP-based solid phase extraction (SPE method gave linear response in the range of 0.05–5.0 mg·L−1 with a detection limit of 9.1 µg·L−1. Finally, the proposed method was used for the selective isolation and enrichment of ST in food samples with recoveries in the range 80.6–88.7% and the relative standard deviation (RSD <5.6%.

  19. Form-Stable Phase Change Materials Based on Eutectic Mixture of Tetradecanol and Fatty Acids for Building Energy Storage: Preparation and Performance Analysis.

    Science.gov (United States)

    Huang, Jingyu; Lu, Shilei; Kong, Xiangfei; Liu, Shangbao; Li, Yiran

    2013-10-22

    This paper is focused on preparation and performance analysis of a series of form-stable phase change materials (FSPCMs), based on eutectic mixtures as phase change materials (PCMs) for thermal energy storage and high-density polyethylene (HDPE)-ethylene-vinyl acetate (EVA) polymer as supporting materials. The PCMs were eutectic mixtures of tetradecanol (TD)-capric acid (CA), TD-lauric acid (LA), and TD-myristic acid (MA), which were rarely explored before. Thermal properties of eutectic mixtures and FSPCMs were measured by differential scanning calorimeter (DSC). The onset melting/solidification temperatures of form-stable PCMs were 19.13 °C/13.32 °C (FS TD-CA PCM), 24.53 °C/24.92 °C (FS TD-LA PCM), and 33.15 °C/30.72 °C (FS TD-MA PCM), respectively, and latent heats were almost greater than 90 J/g. The surface morphologies and chemical stability of form-stable PCM were surveyed by scanning electron microscopy (SEM) and Fourier-transform infrared (FT-IR) spectroscopy, respectively. The thermal cycling test revealed that the thermal reliability of these three form-stable PCMs was good. Thermal storage/release experiment indicated melting/solidification time was shortened by introducing 10 wt % aluminum powder (AP). It is concluded that these FSPCMs can act as potential building thermal storage materials in terms of their satisfactory thermal properties.

  20. Preparation, Mechanical and Thermal Properties of Cement Board with Expanded Perlite Based Composite Phase Change Material for Improving Buildings Thermal Behavior.

    Science.gov (United States)

    Ye, Rongda; Fang, Xiaoming; Zhang, Zhengguo; Gao, Xuenong

    2015-11-13

    Here we demonstrate the mechanical properties, thermal conductivity, and thermal energy storage performance of construction elements made of cement and form-stable PCM-Rubitherm® RT 28 HC (RT28)/expanded perlite (EP) composite phase change materials (PCMs). The composite PCMs were prepared by adsorbing RT28 into the pores of EP, in which the mass fraction of RT28 should be limited to be no more than 40 wt %. The adsorbed RT28 is observed to be uniformly confined into the pores of EP. The phase change temperatures of the RT28/EP composite PCMs are very close to that of the pure RT28. The apparent density and compression strength of the composite cubes increase linearly with the mass fraction of RT28. Compared with the thermal conductivity of the boards composed of cement and EP, the thermal conductivities of the composite boards containing RT28 increase by 15%-35% with the mass fraction increasing of RT28. The cubic test rooms that consist of six boards were built to evaluate the thermal energy storage performance, it is found that the maximum temperature different between the outside surface of the top board with the indoor temperature using the composite boards is 13.3 °C higher than that of the boards containing no RT28. The thermal mass increase of the built environment due to the application of composite boards can contribute to improving the indoor thermal comfort and reducing the energy consumption in the buildings.

  1. Preparation and Thermal Properties of Molecular-Bridged Expanded Graphite/Polyethylene Glycol Composite Phase Change Materials for Building Energy Conservation.

    Science.gov (United States)

    Zhang, Dong; Chen, Meizhu; Liu, Quantao; Wan, Jiuming; Hu, Jinxuan

    2018-05-16

    Using phase change materials (PCMs) in building envelopes became a reliable method to improve indoor comfort and reduce buildings' energy consumption. This research developed molecular-bridged expanded graphite (EG)/polyethylene glycol (PEG) composite PCMs (m-EPs) to conserve energy in buildings. The m-EPs were prepared through a vacuum absorption technique, and a titanate coupling agent was used to build a molecular bridge between EG and PEG. SEM, mercury intrusion porosimetry (MIP), the leakage test, microcalorimetry, X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FT-IR) were conducted to characterize the morphology, pore structure, absorbability, and modifying effects of the m-EPs. The phase change temperature, latent heat, thermal stability, and thermal conductivity of the m-EPs were determined by a differential scanning calorimeter (DSC), TGA, and a thermal constants analyzer. Results showed that the maximum mass ratio of PEG to EG without leakage was 1:7, and a stable connection was established in the m-EPs after modification. Compared with the unmodified EPs, the supercooling degree of the m-EPs reduced by about 3 °C, but the latent heats and initial decomposition temperatures increased by approximately 10% and 20 °C, respectively, which indicated an improvement in the thermal energy storage efficiency. The thermal conductivities of the m-EPs were 10 times higher than those of the pristine PEGs, which ensured a rapid responding to building temperature fluctuations.

  2. Two-stage preparation of magnetic sorbent based on exfoliated graphite with ferrite phases for sorption of oil and liquid hydrocarbons from the water surface

    Science.gov (United States)

    Pavlova, Julia A.; Ivanov, Andrei V.; Maksimova, Natalia V.; Pokholok, Konstantin V.; Vasiliev, Alexander V.; Malakho, Artem P.; Avdeev, Victor V.

    2018-05-01

    Due to the macropore structure and the hydrophobic properties, exfoliated graphite (EG) is considered as a perspective sorbent for oil and liquid hydrocarbons from the water surface. However, there is the problem of EG collection from the water surface. One of the solutions is the modification of EG by a magnetic compound and the collection of EG with sorbed oil using the magnetic field. In this work, the method of the two-stage preparation of exfoliated graphite with ferrite phases is proposed. This method includes the impregnation of expandable graphite in the mixed solution of iron (III) chloride and cobalt (II) or nickel (II) nitrate in the first stage and the thermal exfoliation of impregnated expandable graphite with the formation of exfoliated graphite containing cobalt and nickel ferrites in the second stage. Such two-stage method makes it possible to obtain the sorbent based on EG modified by ferrimagnetic phases with high sorption capacity toward oil (up to 45-51 g/g) and high saturation magnetization (up to 42 emu/g). On the other hand, this method allows to produce the magnetic sorbent in a short period of time (up to 10 s) during which the thermal exfoliation is carried out in the air atmosphere.

  3. Paraffin/expanded graphite phase change composites with enhanced thermal conductivity prepared by implanted β-SiC nanowires with chemical vapor deposition method

    Science.gov (United States)

    Yin, Zhaoyu; Zhang, Xiaoguang; Huang, Zhaohui; Liu, Silin; Zhang, Weiyi; Liu, Yan'gai; Wu, Xiaowen; Fang, Minghao; Min, Xin

    2018-02-01

    Expanded graphite/β-SiC nanowires composites (ESNC) were prepared through chemical vapor deposition, and paraffin/expanded graphite/β-SiC nanowires composites (PESNC) were made through vacuum impregnation to overcome liquid leakage during phase transition and enhance the thermal conductivity of paraffin. Fourier transform infrared spectroscopy showed no chemical interactions between the paraffin and ESNC. Differential scanning calorimetry estimated the temperature and latent heat of PESNC during melting to 45.73 °C and 124.31 J g-1, respectively. The respective values of these quantities during freezing were recorded as 48.93 °C and 124.14 J g-1. The thermal conductivity of PESNC was estimated to 0.75 W mK-1, which was 3.26-folds that of pure paraffin (0.23 W mK-1). PESNC perfectly maintained its phase transition after 200 melting-freezing cycles. The resulting ideal thermal conductivity, good chemical stability, thermal properties and thermal reliability of PESNC are promising for use in energy efficient buildings and solar energy systems.

  4. Two-Phase Diffusion Technique for the Preparation of Ultramacroporous/Mesoporous Silica Microspheres via Interface Hydrolysis, Diffusion, and Gelation of TEOS.

    Science.gov (United States)

    Ju, Minhua; Li, Yupeng; Yu, Liang; Wang, Chongqing; Zhang, Lixiong

    2018-02-06

    Honeycombed hierarchical ultramacroporous/mesoporous silica microspheres were prepared via the hydrolysis of TEOS in the oil-water interface, with subsequent diffusion and gelation in the acidic water-phase microdroplets with the assistance of a simple homemade microdevice. The diffusion of furfuryl alcohol (FA) also happened at a relatively high rate during the hydrolysis and diffusion of TEOS. Therefore, plenty of FA will be inside of the water microdroplets and form a decent number of polyfurfuryl alcohol (PFA) microparticles, thereby obtaining honeycombed hierarchical porosity silica microspheres with abundant ultramacroporous cavities and mesopores after calcination. It was found that the concentration of FA, residence time, and reaction temperature have significant effects on the porosity and pore size due to the influence on the diffusion rate and amount of FA in water-phase microdroplets. The honeycombed silica microspheres have obvious microscopic visible ultramacroporous cavities with the submicrometer cavity diameter as high as 85% porosity based on the rough overall volume of microsphere. N 2 adsorption-desorption isotherms show that the honeycombed hierarchical porosity silica microspheres have a high surface area of 602 m 2 g -1 , a mesopore volume of 0.77 cm 3 /g, and a mesopore porosity of 99.6% based on the total pore volume of N 2 adsorption-desorption. On the basis of the experiment results, a rational formation process of the honeycombed hierarchical porosity silica microspheres was deduced.

  5. The effects of processing conditions on the surface morphology and hydrophobicity of polyvinylidene fluoride membranes prepared via vapor-induced phase separation

    Science.gov (United States)

    Peng, Yuelian; Fan, Hongwei; Ge, Ju; Wang, Shaobin; Chen, Ping; Jiang, Qi

    2012-12-01

    The present investigation reveals how the surface morphology and the hydrophobicity of polyvinylidene fluoride (PVDF) membranes, which were prepared via a vapor-induced phase separation method, were affected by the initial PVDF content in the casting solution and the air temperature. The surface morphology was characterized with scanning electron microscopy. A ternary phase diagram of PVDF/N, N-dimethylacetamide/water was constructed to explain the formation mechanism of the different morphologies. The results show that different membrane morphologies and hydrophobicities can be obtained by changing the processing conditions. Low air temperature and high PVDF contents facilitate the crystallization process, resulting in the formation of a porous skin and particle morphology, which increases the hydrophobicity of the surface. High air temperature and low PVDF contents are favorable for the formation of a net-like surface morphology via spinodal decomposition and lead to a superhydrophobic surface. Theoretical calculations were performed to testify that the net-like surface was more favorable for superhydrophobicity than the particle-based surface.

  6. Preparation and characterizations of HDPE-EVA alloy/OMT nanocomposites/paraffin compounds as a shape stabilized phase change thermal energy storage material

    International Nuclear Information System (INIS)

    Cai Yibing; Hu Yuan; Song Lei; Lu Hongdian; Chen Zuyao; Fan Weicheng

    2006-01-01

    A kind of shape stabilized phase change nanocomposites materials (PCNM) based on high density polyethylene (HDPE)/ethylene-vinyl acetate (EVA) alloy, organophilic montmorillonite (OMT), paraffin and intumescent flame retardant (IFR) are prepared using twin-screw extruder technique. The structures of the HDPE-EVA alloy/OMT nanocomposites are evidenced by the X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that an ordered intercalated nanomorphology of the HDPE-EVA alloy/OMT nanocomposites is formed. Then the structures of the shape stabilized PCNM are characterized by scanning electron microscopy (SEM). The HDPE-EVA alloy/OMT nanocomposites act as the supporting material and form the three-dimensional network structure. The paraffin acts as a phase change material and disperses in the three-dimensional network structure. Its latent heat is given by differential scanning calorimeter (DSC) method. The SEM and DSC results show that the additives of IFR have little effect on the network structure and the latent heat of shape stabilized PCNM, respectively. The thermal stability properties are characterized by thermogravimetric analysis (TGA). The TGA analysis results indicate that the flame retardant shape stabilized PCNM produce a larger amount of char residue at 800 deg. C than that of shape stabilized PCNM, although the onset of weight loss of the flame retardant shape stabilized PCNM occur at a lower temperature. The formed multicellular char residue contributes to the improvement of thermal stability performance. The probable combustion mechanisms are also discussed in this paper

  7. Annotated bibliography on selected areas of coal mining research and development. Report prepared for the Committee on Science and Technology, US House of Representatives, Ninety-Sixth Congress, First Session by the Congressional Research Service, Library of Congress

    Energy Technology Data Exchange (ETDEWEB)

    1979-01-01

    The Congressional Research Service has completed an annotated bibliography on coal mining research and development. Although the completion of the study was delayed in order to permit CRS analysts to search the libraries of Bituminous Coal, Research Inc., and the Bureau of Mines in the Pittsburgh area, current re-emphasis on the use of coal as an energy source indicates a sustained relevance. The bibliography presents key references to coal-mining R and D under six subject headings keyed to issues of central concern in coal production: (1) mine health and safety, (2) methane recovery, (3) 1-hour rescuer, (4) use of diesels underground, (5) coal preparation, and (6) manpower development in coal mining.

  8. Structural Analyses of Phase Stability in Amorphous and Partially Crystallized Ge-Rich GeTe Films Prepared by Atomic Layer Deposition.

    Science.gov (United States)

    Gwon, Taehong; Mohamed, Ahmed Yousef; Yoo, Chanyoung; Park, Eui-Sang; Kim, Sanggyun; Yoo, Sijung; Lee, Han-Koo; Cho, Deok-Yong; Hwang, Cheol Seong

    2017-11-29

    The local bonding structures of Ge x Te 1-x (x = 0.5, 0.6, and 0.7) films prepared through atomic layer deposition (ALD) with Ge(N(Si(CH 3 ) 3 ) 2 ) 2 and ((CH 3 ) 3 Si) 2 Te precursors were investigated using Ge K-edge X-ray absorption spectroscopy (XAS). The results of the X-ray absorption fine structure analyses show that for all of the compositions, the as-grown films were amorphous with a tetrahedral Ge coordination of a mixture of Ge-Te and Ge-Ge bonds but without any signature of Ge-GeTe decomposition. The compositional evolution in the valence band electronic structures probed through X-ray photoelectron spectroscopy suggests a substantial chemical influence of additional Ge on the nonstoichiometric GeTe. This implies that the ALD process can stabilize Ge-abundant bonding networks like -Te-Ge-Ge-Te- in amorphous GeTe. Meanwhile, the XAS results on the Ge-rich films that had undergone post-deposition annealing at 350 °C show that the parts of the crystalline Ge-rich GeTe became separated into Ge crystallites and rhombohedral GeTe in accordance with the bulk phase diagram, whereas the disordered GeTe domains still remained, consistent with the observations of transmission electron microscopy and Raman spectroscopy. Therefore, amorphousness in GeTe may be essential for the nonsegregated Ge-rich phases and the low growth temperature of the ALD enables the achievement of the structurally metastable phases.

  9. Preparation and Supercooling Modification of Salt Hydrate Phase Change Materials Based on CaCl₂·2H₂O/CaCl₂.

    Science.gov (United States)

    Xu, Xiaoxiao; Dong, Zhijun; Memon, Shazim Ali; Bao, Xiaohua; Cui, Hongzhi

    2017-06-23

    Salt hydrates have issues of supercooling when they are utilized as phase change materials (PCMs). In this research, a new method was adopted to prepare a salt hydrate PCM (based on a mixture of calcium chloride dihydrate and calcium chloride anhydrous) as a novel PCM system to reduce the supercooling phenomenon existing in CaCl₂·6H₂O. Six samples with different compositions of CaCl₂ were prepared. The relationship between the performance and the proportion of calcium chloride dihydrate (CaCl₂·2H₂O) and calcium chloride anhydrous (CaCl₂) was also investigated. The supercooling degree of the final PCM reduced with the increase in volume of CaCl₂·2H₂O during its preparation. The PCM obtained with 66.21 wt % CaCl₂·2H₂O reduced the supercooling degree by about 96.8%. All six samples, whose ratio of CaCl₂·2H₂O to (CaCl₂ plus CaCl₂·2H₂O) was 0%, 34.03%, 53.82%, 76.56%, 90.74%, and 100% respectively, showed relatively higher enthalpy (greater than 155.29 J/g), and have the possibility to be applied in buildings for thermal energy storage purposes. Hence, CaCl₂·2H₂O plays an important role in reducing supercooling and it can be helpful in adjusting the solidification enthalpy. Thereafter, the influence of adding different percentages of Nano-SiO₂ (0.1 wt %, 0.3 wt %, 0.5 wt %) in reducing the supercooling degree of some PCM samples was investigated. The test results showed that the supercooling of the salt hydrate PCM in Samples 6 and 5 reduced to 0.2 °C and 0.4 °C respectively. Finally, the effect of the different cooling conditions, including frozen storage (-20 °C) and cold storage (5 °C), that were used to prepare the salt hydrate PCM was considered. It was found that both cooling conditions are effective in reducing the supercooling degree of the salt hydrate PCM. With the synergistic action of the two materials, the performance and properties of the newly developed PCM systems were better especially in terms of reducing

  10. Application of colloidal chemistry in aqueous phase to the preparation of supported metallic catalysts: particles size and aggregation control; Application de la chimie colloidale en phase aqueuse a la preparation de catalyseurs metalliques supportes: controle de la taille et de l`etat d`agregation des particules

    Energy Technology Data Exchange (ETDEWEB)

    Pages, T.

    1998-09-16

    This work is an application of colloidal chemistry in aqueous phase on supported metal catalyst preparation. The objective is the control of particle size and aggregation. The preparation of the materials was achieved in two steps: - the synthesis of PdO hydrosols was obtained by two ways: neutralisation of the solution containing metallic salt by adding alkaline solution or by thermo-hydrolysis; the sols were then deposited on carriers (Al{sub 2}O{sub 3}, SIO{sub 2}). The use of partial charge model allowed us to determine the complexes that were able to generate PdO. The preparation of PdO from Pd(H{sub 2}O){sub 4}{sup 2+} was studied and a mechanism of oxide formation was elaborated. The neutralisation of Pd(H{sub 2}O){sub 4}{sup 2+} obtained by adding alkaline solution led to particles with an average size of 1.8 nm and a narrow particle size distribution. Only the thermo-hydrolysis of Pd(H{sub 2}O){sub 4}{sup 2+} led to particles which size is higher than 3.0 nm. In the last case, particle size is controlled by the precursor concentration (Pd(H{sub 2}O){sub 2}(OH){sub 2}) generated in the medium. We have demonstrated that particle aggregation in the sol depends on the Ph and the way of preparation. It can be controlled by adding complexing anions (Cl{sup -}, NO{sub 2}{sup -}). Concerning the deposition of sols on carriers, it led to isolated or aggregated particles according to experimental conditions. Particle size was not modified during the deposition. Moreover, in our experimental conditions, reduction of particles did not modify particle size and aggregation. An application of this original way of preparation on catalysis allowed us to demonstrate the interest of controlling particle size and aggregation. (author) 186 refs.

  11. List of Accredited Representatives

    Data.gov (United States)

    Department of Veterans Affairs — VA accreditation is for the sole purpose of providing representation services to claimants before VA and does not imply that a representative is qualified to provide...

  12. In-situ transmission electron microscopy of the solid-phase epitaxial growth of GaAs: sample preparation and artifact characterization

    International Nuclear Information System (INIS)

    Llewellyn, D.J.; Llewellyn, D.J.; Belay, K.B.; Ridgway, M.C.

    1998-01-01

    In-situ transmission electron microscopy (TEM) has been used to characterize the solid phase epitaxial growth of amorphized GaAs at a temperature of 260 deg C. To maximize heat transfer from the heated holder to the sample and minimize electron-irradiation induced artifacts, non-conventional methodologies were utilized for the preparation of cross-sectional samples. GaAs 3x1 mm rectangular wafers were cleaved then glued face-to-face to form a wafer stack size of 3x3 mm while maintaining the TEM region at the center. This stack was subsequently polished on the cross-section to a thickness of ∼ 200 μm. A 3 mm disc was then cut perpendicular to the cross-section using a Gatan ultrasonic cutter. The disc was polished then dimpled on both sides to a thickness of ∼ 15 μm. This was ion-beam milled at liquid nitrogen temperature to an electron-transparent layer. From a comparison of in-situ and ex-situ measurements of the recrystallization rate, the actual sample temperature during in-situ characterization was estimated to deviate by ≤ 20 deg C from that of the heated holder. The influence of electron-irradiation was found to be negligible by comparing the recrystallization rate and microstructure of irradiated and unirradiated regions of comparable thickness. Similarly, the influence of the 'thin-foil effect' was found to be negligible by comparing the recrystallization rate and microstructure of thick and thin regions, the former determined after the removal of the sample from the microscope and further ion-beam milling of tens of microns of material. In conclusion, the potential influence of artifacts during in-situ TEM can be minimized by the appropriate choice of sample preparation procedures. (authors)

  13. Thermoelectric Properties of Cu-Doped n-Type Bi2Te2.85Se0.15 Prepared by Liquid Phase Growth Using a Sliding Boat

    Science.gov (United States)

    Kitagawa, Hiroyuki; Matsuura, Tsukasa; Kato, Toshihito; Kamata, Kin-ya

    2015-06-01

    N-type Bi2Te2.85Se0.15 thermoelectric materials were prepared by liquid phase growth (LPG) using a sliding boat, a simple and short fabrication process for Bi2Te3-related materials. Cu was selected as a donor dopant, and its effect on thermoelectric properties was investigated. Thick sheets and bars of Cu x Bi2 Te2.85Se0.15 ( x=0-0.25) of 1-2mm in thickness were obtained using the process. X-ray diffraction patterns and scanning electron micrographs showed that the in-plane direction tended to correspond to the hexagonal c-plane, which is the preferred direction for thermoelectric conversion. Cu-doping was effective in controlling conduction type and carrier (electron) concentration. The conduction type was p-type for undoped Bi2Te2.85Se0.15 and became n-type after Cu-doping. The Hall carrier concentration was increased by Cu-doping. Small resistivity was achieved in Cu0.02Bi2Te2.85Se0.15 owing to an optimized amount of Cu-doping and high crystal orientation. As a result, the maximum power factor near 310K for Cu0.02Bi2Te2.85Se0.15 was approximately 4×10-3W/K2m and had good reproducibility. Furthermore, the thermal stability of Cu0.02Bi2Te2.85Se0.15 was also confirmed by thermal cycling measurements of electrical resistivity. Thus, n-type Bi2Te2.85Se0.15 with a large power factor was prepared using the present LPG process.

  14. Preparation of silica-supported carbon by Kraft lignin pyrolysis, and its use in solid-phase extraction of fluoroquinolones from environmental waters

    International Nuclear Information System (INIS)

    Speltini, Andrea; Sturini, Michela; Maraschi, Federica; Mandelli, Elettra; Dondi, Daniele; Profumo, Antonella; Vadivel, Dhanalakshmi

    2016-01-01

    The article describes a carbon-based material for solid-phase extraction (SPE) of fluoroquinolones from waters. It was obtained by pyrolytic deposition of Kraft lignin (LG) on silica particles. Marbofloxacin (MAR) and enrofloxacin (ENR) were chosen as model contaminants. The material was prepared by first adsorbing LG onto silica microparticles, this followed by pyrolytic treatment at 1200 °C for 2 h. Silica-supported carbon was characterized by scanning electron microscopy, surface area measurement (by BET), thermogravimetric analysis, and electron paramagnetic resonance. The carbon-coated silica particles were then tested as a column packing for SPE of MAR and ENR from spiked tap and river waters. Quantitative adsorption was observed at pH values of ∼7.5 for both drugs. They were eluted with a 70:30 mixture of aqueous tetrabutylammonium hydroxide and acetonitrile and then quantified by HPLC coupled to fluorescence detection. Samples spiked with MAR and ENR in the range from 10 to 1000 ng·L"−"1 gave recoveries ranging from 70 to 116% (for n = 3). Good inter-day precision (with RSDs between 7 and 16%) was observed for 20–1000 ng·L"−"1 spikes, also in natural river water. Sample volumes up to 500 mL provided enrichment factors up to 125, and this makes this material useful for determination of the two drugs at environmentally significant levels which are as low as a few ng·L"−"1. The batch-to-batch reproducibility was verified for 3 preparations. The sorbent was successfully applied to the determination of these drugs in environmental waters. (author)

  15. Molecularly imprinted polymer microspheres prepared by Pickering emulsion polymerization for selective solid-phase extraction of eight bisphenols from human urine samples

    International Nuclear Information System (INIS)

    Yang, Jiajia; Li, Yun; Wang, Jincheng; Sun, Xiaoli; Cao, Rong; Sun, Hao; Huang, Chaonan; Chen, Jiping

    2015-01-01

    Highlights: • BPA imprinted polymer microspheres were prepared by Pickering emulsion polymerization. • Regular spherical shape and narrow diameter distribution. • Good specific adsorption capacity for BPA. • Good class-selectivity and clean-up efficiency for bisphenols in human urine under SPE mode. • Good recoveries and sensitivity for bisphenols using the MIPMS-SPE coupled with HPLC-DAD method. - Abstract: The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption–desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30–60 μm), a specific surface area (S BET ) of 281.26 m 2 g −1 and a total pore volume (V t ) of 0.459 cm 3 g −1 . Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2–2.2 ng mL −1 . The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL −1 for each BP) were in the range of 81.3–106.7% with RSD values below 8.3%

  16. An Exploration into the Bacterial Community under Different Pasteurization Conditions during Substrate Preparation (Composting-Phase II) for Agaricus bisporus Cultivation.

    Science.gov (United States)

    Vieira, Fabricio Rocha; Pecchia, John Andrew

    2018-02-01

    Substrate preparation (i.e., composting) for Agaricus bisporus cultivation is the most critical point of mushroom production. Among many factors involved in the composting process, the microbial ecology of the system is the underlying drive of composting and can be influenced by composting management techniques. Pasteurization temperature at the beginning of phase II, in theory, may influence the bacterial community and subsequently the "selectivity" and nutrition of the final substrate. Therefore, this hypothesis was tested by simulation in bioreactors under different pasteurization conditions (57 °C/6 h, 60 °C/2 h, and 68 °C/2 h), simulating conditions adopted by many producers. Bacterial diversity, based on 16S ribosomal RNA obtained by high-throughput sequencing and classified in operational taxonomic units (OTUs), was greater than previously reported using culture-dependent methods. Alpha diversity estimators show a lower diversity of OTUs under a high-temperature pasteurization condition. Bacillales order shows a relatively higher OTU abundance under a high-pasteurization temperature, which also was related to high ammonia emission measurements. On the other hand, beta diversity analysis showed no significantly changes in the bacterial community structure under different conditions. Agaricus bisporus mycelium growth during a standard spawn run period was significantly slower in the compost pasteurized at high temperature. Since the bacterial community structure was not greatly affected by different pasteurization conditions but by-products left (e.g., ammonia) at the end of compost conditioning varied, further studies need to be conducted to determine the functional role of the microbial communities found during substrate preparation for Agaricus bisporus cultivation.

  17. On the solid phase crystallization of In{sub 2}O{sub 3}:H transparent conductive oxide films prepared by atomic layer deposition

    Energy Technology Data Exchange (ETDEWEB)

    Macco, Bart; Verheijen, Marcel A.; Black, Lachlan E.; Melskens, J. [Department of Applied Physics, Eindhoven University of Technology, P.O. Box 513, 5600 MB Eindhoven (Netherlands); Barcones, Beatriz [NanoLab@TU/e, Eindhoven University of Technology, P.O. Box 513, 5600 MB Eindhoven (Netherlands); Kessels, Wilhelmus M. M., E-mail: w.m.m.kessels@tue.nl [Department of Applied Physics, Eindhoven University of Technology, P.O. Box 513, 5600 MB Eindhoven (Netherlands); Solliance Solar Research, High Tech Campus 5, 5656 AE Eindhoven (Netherlands)

    2016-08-28

    Hydrogen-doped indium oxide (In{sub 2}O{sub 3}:H) has emerged as a highly transparent and conductive oxide, finding its application in a multitude of optoelectronic devices. Recently, we have reported on an atomic layer deposition (ALD) process to prepare high quality In{sub 2}O{sub 3}:H. This process consists of ALD of In{sub 2}O{sub 3}:H films at 100 °C, followed by a solid phase crystallization step at 150–200 °C. In this work, we report on a detailed electron microscopy study of this crystallization process which reveals new insights into the crucial aspects for achieving the large grain size and associated excellent properties of the material. The key finding is that the best optoelectronic properties are obtained by preparing the films at the lowest possible temperature prior to post-deposition annealing. Electron microscopy imaging shows that such films are mostly amorphous, but feature a very low density of embedded crystallites. Upon post-deposition annealing, crystallization proceeds merely from isotropic crystal grain growth of these embedded crystallites rather than by the formation of additional crystallites. The relatively high hydrogen content of 4.2 at. % in these films is thought to cause the absence of additional nucleation, thereby rendering the final grain size and optoelectronic properties solely dependent on the density of embedded crystallites. The temperature-dependent grain growth rate has been determined, from which an activation energy of (1.39 ± 0.04) eV has been extracted. Finally, on the basis of the observed crystallization mechanism, a simple model to fully describe the crystallization process has been developed. This model has been validated with a numerical implementation thereof, which accurately predicts the observed temperature-dependent crystallization behaviour.

  18. Preparation and properties of palmitic-stearic acid eutectic mixture/expanded graphite composite as phase change material for energy storage

    International Nuclear Information System (INIS)

    Zhang, Nan; Yuan, Yanping; Du, Yanxia; Cao, Xiaoling; Yuan, Yaguang

    2014-01-01

    A novel composite PCM (phase change material) with PA-SA (palmitic-stearic acid) eutectic mixture as PCM and EG (expanded graphite) as supporting material was prepared. The optimum absorption ratio of PA-SA/EG (Palmitic-stearic acid/expanded graphite) composite PCM was determined as PA-SA:EG = 13:1 (by mass). Scanning electron microscope and Fourier transformation infrared spectroscopy results show that PA-SA was uniformly distributed in the porous network structure of EG due to the physical action. Thermal property and thermal stability of the PA-SA/EG composite PCM were characterized by DSC (differential scanning calorimetry) and TGA (thermogravimetric analysis). DSC results indicated that the melting and freezing temperatures and latent heats of PA-SA/EG were measured as 53.89 °C and 54.37 °C, and 166.27 J/g and 166.13 J/g. TGA test results revealed that PA-SA/EG had a good thermal stability in working temperature range. Thermal cycling test results showed PA-SA/EG had a good thermal reliability after 720 thermal cycles. Thermal conductivity of the composite PCM was measured as 2.51 W/m K, much higher than that of PA-SA. The thermal energy storage and release rates of PA-SA/EG were also increased due to the high thermal conductivity of EG. In conclusion, the prepared PA-SA/EG composite PCM can be acted as a potential material for thermal energy storage due to the acceptable thermal properties, good thermal reliability and stability, high thermal conductivity. - Highlights: • PA-SA/EG (Palmitic-stearic acid/expanded graphite) composite PCM was prepared. • Optimum absorption ratio of PA-SA in EG was obtained as 13:1 (by mass). • Thermal conductivity and performance of PA-SA/EG have been significate improved. • PA-SA/EG has a good thermal reliability and thermal stability

  19. Preparation and properties studies of halogen-free flame retardant form-stable phase change materials based on paraffin/high density polyethylene composites

    International Nuclear Information System (INIS)

    Cai Yibing; Wei Qufu; Huang Fenglin; Gao Weidong

    2008-01-01

    The halogen-free flame retardant form-stable phase change materials (PCM) based on paraffin/high density polyethylene (HDPE) composites were prepared by using twin-screw extruder technique. The structures and properties of the form-stable PCM composites based on intumescent flame retardant system with expandable graphite (EG) and different synergistic additives, such as ammonium polyphosphate (APP) and zinc borate (ZB) were characterized by scanning electronic microscope (SEM), thermogravimetric analyses (TGA), dynamic Fourier-transform infrared (FTIR) spectra, differential scanning calorimeter (DSC) and Cone calorimeter test. The TGA results showed that the halogen-free flame retardant form-stable PCM composites produced a larger amount of charred residue at 700 deg. C, although the onset of weight loss of the halogen-free flame retardant form-stable PCM composites occurred at a lower temperature due to the thermal decomposition of flame retardant. The DSC measurements indicated that the additives of flame retardant had little effect on the thermal energy storage property, and the temperatures of phase change peaks and the latent heat of the paraffin showed better occurrence during the freezing process. The dynamic FTIR monitoring results revealed that the breakdowns of main chains (HDPE and paraffin) and formations of various residues increased with increasing thermo-oxidation temperature. It was also found from the Cone calorimeter tests that the peak of heat release rate (PHRR) decreased significantly. Both the decrease of the PHRR and the structure of charred residue after combustion indicated that there was a synergistic effect between the EG and APP, contributing to the improved flammability of the halogen-free flame retardant form-stable PCM composites

  20. Preparation of poly(trimethyl-2-methacroyloxyethylammonium chloride-co-ethylene glycol dimethacrylate) monolith and its application in solid phase microextraction of brominated flame retardants.

    Science.gov (United States)

    Yang, Ting-ting; Zhou, Lin-feng; Qiao, Jun-qin; Lian, Hong-zhen; Ge, Xin; Chen, Hong-yuan

    2013-05-24

    A capillary poly(trimethyl-2-methacroyloxyethylammonium chloride-co-ethylene glycol dimethacrylate) monolith was in situ synthesized by thermally initiated free radical co-polymerization using trimethyl-2-methacroyloxyethylammonium chloride (MATE) and ethylene glycol dimethacrylate (EGDMA) as functional monomer and cross-linker, respectively. N,N-dimethylformamide and polyethylene glycol 6000 were used as solvent and porogen, respectively. The morphology and porous structure of the resulting monoliths were assessed by scanning electron microscope. In order to prepare practically useful poly(MATE-co-EGDMA) monoliths with low flow resistance and good mechanical strength, some parameters such as PEG-6000 to DMF ratio, total monomer to porogen ratio, and crosslinker to monomer ratio were optimized systematically. Moreover, the extraction mechanism was evaluated using two series of compounds, alkylbenzenes and weak acids, as model compounds on poly(MATE-co-EGDMA) monoliths as liquid chromatographic stationary phase. Finally, the monoliths were applied as the solid phase microextraction medium, and a simple off-line method for simultaneous determination of three brominated flame retardants, 2,4,6-tribromophenol (TBP), tetrabromobisphenol A (TBBPA) and 4,4'-dibrominated diphenyl ether (DBDPE), in environmental waters was developed by coupling the polymer monolith microextraction to HPLC with UV detection. The regression equations for these three brominated flame retardants showed good linearity from their limit of quantification to 5000ng/mL. The limits of detection were 0.20, 0.15 and 0.10ng/mL for TBP, TBBPA and DBDPE, respectively. The recovery of the proposed method was 78.7-106.1% with intra-day relative standard deviation of 1.3-4.4%. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib, E-mail: bagheri@sharif.edu [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of); Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2012-02-24

    A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2-10 ng L{sup -1}. The relative standard deviations (RSD) (n = 3) at the concentration level of 1.7-6.7 ng mL{sup -1} were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27-1330 ng L{sup -1} for phenol and monochlorophenols and 7-1000 ng L{sup -1} for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%.

  2. Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

    International Nuclear Information System (INIS)

    Bagheri, Habib; Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza

    2012-01-01

    A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100–200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography–mass spectrometry (GC–MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2–10 ng L −1 . The relative standard deviations (RSD) (n = 3) at the concentration level of 1.7–6.7 ng mL −1 were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27–1330 ng L −1 for phenol and monochlorophenols and 7–1000 ng L −1 for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%.

  3. Artificially phase-separated binary self-assembled monolayers composed of 11-amino-1-undecanethiolate and 10-carboxy-1-decanethiolate on Au(1 1 1): A comparative study of two preparing methods

    International Nuclear Information System (INIS)

    Phong, Pham Hong; Tomono, Hyroyuki; Nishi, Naoya; Yamamoto, Masahiro; Kakiuchi, Takashi

    2008-01-01

    Two methods have been compared for preparing artificially phase-separated two-component SAMs on Au(1 1 1) composed of 11-amino-1-undecanethiolates (AUTe) and 10-carboxyl-1-decanethiolates (CDTe), which would form, thermodynamically, a homogeneously mixed binary SAMs. The first method starts with the formation of a phase-separated binary SAM of AUTe and 2-hydroxy-1-ethanethiolate (HETe) as a template of the artificially phase-separated SAM, followed by the selective desorption of HETe domains and succeeding filling of the vacancy with CDTe. The second method utilizes fluoren-9-ylmethyl N-(11-mercaptoundecyl) carbamate (FMUCe) instead of 11-amino-1-undecanethiol in preparing the template. After the filling with CDTe, the 9-fluorenylmethyloxycarbonyl (Fmoc) group is removed to obtain AUTe domains. Both methods yield artificially phase-separated binary SAMs having AUTe domains of tens nanometer across. The molecularly flat SAM surface with nanometer-scale domains of different acid-base and electrostatic properties are thus created. For preparing binary SAMs with a higher degree of phase separation, the second method is a better choice; a more clear-cut phase separation is achieved

  4. Representing vision and blindness.

    Science.gov (United States)

    Ray, Patrick L; Cox, Alexander P; Jensen, Mark; Allen, Travis; Duncan, William; Diehl, Alexander D

    2016-01-01

    There have been relatively few attempts to represent vision or blindness ontologically. This is unsurprising as the related phenomena of sight and blindness are difficult to represent ontologically for a variety of reasons. Blindness has escaped ontological capture at least in part because: blindness or the employment of the term 'blindness' seems to vary from context to context, blindness can present in a myriad of types and degrees, and there is no precedent for representing complex phenomena such as blindness. We explore current attempts to represent vision or blindness, and show how these attempts fail at representing subtypes of blindness (viz., color blindness, flash blindness, and inattentional blindness). We examine the results found through a review of current attempts and identify where they have failed. By analyzing our test cases of different types of blindness along with the strengths and weaknesses of previous attempts, we have identified the general features of blindness and vision. We propose an ontological solution to represent vision and blindness, which capitalizes on resources afforded to one who utilizes the Basic Formal Ontology as an upper-level ontology. The solution we propose here involves specifying the trigger conditions of a disposition as well as the processes that realize that disposition. Once these are specified we can characterize vision as a function that is realized by certain (in this case) biological processes under a range of triggering conditions. When the range of conditions under which the processes can be realized are reduced beyond a certain threshold, we are able to say that blindness is present. We characterize vision as a function that is realized as a seeing process and blindness as a reduction in the conditions under which the sight function is realized. This solution is desirable because it leverages current features of a major upper-level ontology, accurately captures the phenomenon of blindness, and can be

  5. High mobility In{sub 2}O{sub 3}:H transparent conductive oxides prepared by atomic layer deposition and solid phase crystallization

    Energy Technology Data Exchange (ETDEWEB)

    Macco, B.; Wu, Y.; Vanhemel, D. [Department of Applied Physics, Eindhoven University of Technology (Netherlands); Kessels, W.M.M. [Department of Applied Physics, Eindhoven University of Technology (Netherlands); Solliance Solar Research, Eindhoven (Netherlands)

    2014-12-01

    The preparation of high-quality In{sub 2}O{sub 3}:H, as transparent conductive oxide (TCO), is demonstrated at low temperatures. Amorphous In{sub 2}O{sub 3}:H films were deposited by atomic layer deposition at 100 C, after which they underwent solid phase crystallization by a short anneal at 200 C. TEM analysis has shown that this approach can yield films with a lateral grain size of a few hundred nm, resulting in electron mobility values as high as 138 cm{sup 2}/V s at a device-relevant carrier density of 1.8 x 10{sup 20} cm{sup -3}. Due to the extremely high electron mobility, the crystallized films simultaneously exhibit a very low resistivity (0.27 mΩ cm) and a negligible free carrier absorption. In conjunction with the low temperature processing, this renders these films ideal candidates for front TCO layers in for example silicon heterojunction solar cells and other sensitive optoelectronic applications. (copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  6. Solid-phase radioimmunoassay for Epstein-Barr virus-associated membrane antigen prepared from B95-8 cell culture supernatants

    International Nuclear Information System (INIS)

    Doelken, G.; Klein, G.

    1977-01-01

    Epstein-Barr virus (EBV)-associated membrane antigen (MA) was concentrated from B95-8 cell culture media by precipitation with polyethylene glycol followed by chromatography on Bio-Gel A-50m. In a RAJI cell-binding assay, MA-positive material could only be found in the void volume of the column. After ultracentrifugation all antigenic activity appeared in the pellet, which suggested that MA was present in aggregates, presumably fragments of cellular membranes and/or virus envelopes. The MA-containing preparation was photopolymerized in polyacrylamide gel. The homogenized gel was used in a solid-phase radioimmunoassay with 125 I-labeled IgG from an anti-MA positive reference serum and an anti-MA negative control serum. The specificity of the reaction was confirmed in blocking tests with anti-EBV positive and negative sera. A good correlation was found between the results obtained in the radioimmunoassay and the results obtained in direct immunofluorescence tests for the detection of MA. The existence of at least two subspecificities of the MA complex could be confirmed by this radioimmunoassay

  7. Preparation, characterization, and application of poly(vinyl alcohol)-graft-poly(ethylene glycol) resins: novel polymer matrices for solid-phase synthesis.

    Science.gov (United States)

    Luo, Juntao; Pardin, Christophe; Zhu, X X; Lubell, William D

    2007-01-01

    Spherical crosslinked poly(vinyl alcohol) (PVA) beads with good mechanical stability were prepared by reverse-suspension polymerization, using dimethyl sulfoxide (DMSO) as a cosolvent in an aqueous phase. Poly(ethylene glycol)s with varying chain lengths were grafted onto the PVA beads by anionic polymerization of ethylene oxide. The thermal behavior, morphology, and swelling were evaluated for each of the new polymer matrices. High loading and good swelling in water and organic solvents were characteristic of the PEG-grafted PVA beads. The polymer beads also exhibited good mechanical and chemical stability and were unaffected by treatment with 6 N HCl and with 6 N NaOH. The hydroxyl groups of the PVA-PEG beads were converted into aldehyde, carboxylic acid, and isocyanate functions to provide scavenger resins and were extended by way of a benzyl alcohol in a Wang linker. The transglutaminase substrates dipeptides (Z-Gln-Gly) and heptapeptides (Pro-Asn-Pro-Gln-Leu-Pro-Phe) were synthesized on PVA-PEG_5, PVA-PEG_20, and the Wang linker-derivatized PVA-PEG resins. The cleavage of the peptides from the resins using MeOH/NH3 mixture at different temperatures (0 degrees C and room temp) and 50% TFA/DCM provided, respectively, peptide methyl esters, amides, and acids in good yields and purity as assessed by LC-MS analysis.

  8. Preparation of 1-(2-pyridylazo)-2-naphthol functionalized benzophenone/naphthalene and their uses in solid phase extractive preconcentration/separation of uranium(VI)

    International Nuclear Information System (INIS)

    Preetha, C.R.; Prasada Rao, T.

    2003-01-01

    The preparation of solid reagent 1-(2-pyridylazo)-2-naphthol functionalized benzophenone/naphthalene for preconcentration/separation of uranium(VI) is described. These reagents enriches uranium(VI) quantitatively from dilute aqueous solutions in the pH range 10.5-11.0. The solid mixture consisting of the enriched metal ion along with solid phase extractant were dissolved in 2 ml of acetone and uranium(VI) content was established spectrophotometrically by using Arsenazo III procedure. Calibration graphs were rectilinear over the uranium(VI) concentration in the range 0.002-0.1 μg cm -3 . Five replicate determinations of 40 μg of uranium present in 1 dm 3 of sample solution gave a mean absorbance of 0.185 with a relative standard deviation of 1.4%. The detection limit (corresponding to 3 times the standard deviation of the blank) and the enrichment factor were found to be 2 μg dm -3 and 500 respectively. Further the possible separation of uranium(VI) from several bivalent, trivalent and tetravalent elements was also established. In addition to validating the developed method by successfully analysing marine sediment reference material (MESS-3), uranium content was established in soil, river and marine sediment samples by the developed method and compared with standard inductively coupled plasma mass spectrometry (ICP-MS) values. (orig.)

  9. One-pot preparation of magnetic carbon adsorbent derived from pomelo peel for magnetic solid-phase extraction of pollutants in environmental waters.

    Science.gov (United States)

    Huang, Youfang; Peng, Jinghe; Huang, Xiaojia

    2018-04-20

    In this work, magnetic carbon material derived from pomelo peels (MCMPs) was conveniently fabricated utilizing one-pot synthesis method and employed as adsorbent of magnetic solid-phase extraction (MSPE). Several characterized measures including infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and vibrating sample magnetometer were used to investigate the morphology, spectroscopic and magnetic properties of prepared adsorbent. Apolar parabens and polar fluoroquinolones (FQs) were used to investigate the extraction performance of MCMPs. Under the optimized extraction conditions, the MCMPs displayed satisfactory extraction performance for target analytes. At the same time, the MCMPs/MSPE was combined with HPLC-DAD for the sensitive determination of parabens and FQs in real-life water samples. Results showed that the limits of detection (S/N = 3) for parabens and FQs were in the ranges of 0.011-0.053 μg/L and 0.012-0.46 μg/L, respectively. The spiked recoveries were in the range of 76.6-116% for parabens and 80.2-114% for FQs with good repeatability (relative standard deviations less than 10%). In comparison to reported methods, the developed MCMPs/MSPE-HPLC-DAD showed some merits including low-cost, simplicity, satisfactory sensitivity and green non-pollution. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Phase composition, microstructure, and mechanical properties of porous Ti-Nb-Zr alloys prepared by a two-step foaming powder metallurgy method.

    Science.gov (United States)

    Rao, X; Chu, C L; Zheng, Y Y

    2014-06-01

    Porous Ti-Nb-Zr alloys with different porosities from 6.06 to 62.8% are prepared by a two-step foaming powder metallurgy method using TiH2, Nb, and Zr powders together with 0 to 50wt% of NH4HCO3. The effects of the amounts of Nb and Zr as well as the sintering temperature (1473 to 1673K) on their phase composition, porosity, morphology, and mechanical characteristics are investigated. By controlling the porosity, Nb and Zr concentrations as well as the sintering temperature, porous Ti-Nb-Zr alloys with different mechanical properties can be obtained, for example, the hardness between 290 and 63HV, the compressive strength between 1530.5 and 73.4MPa, and the elastic modulus between 10.8 and 1.2GPa. The mechanical properties of the sintered porous Ti-Nb-Zr alloys can be tailored to match different requirements for the human bones and are thus potentially useful in the hard tissue implants. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. Representing Color Ensembles.

    Science.gov (United States)

    Chetverikov, Andrey; Campana, Gianluca; Kristjánsson, Árni

    2017-10-01

    Colors are rarely uniform, yet little is known about how people represent color distributions. We introduce a new method for studying color ensembles based on intertrial learning in visual search. Participants looked for an oddly colored diamond among diamonds with colors taken from either uniform or Gaussian color distributions. On test trials, the targets had various distances in feature space from the mean of the preceding distractor color distribution. Targets on test trials therefore served as probes into probabilistic representations of distractor colors. Test-trial response times revealed a striking similarity between the physical distribution of colors and their internal representations. The results demonstrate that the visual system represents color ensembles in a more detailed way than previously thought, coding not only mean and variance but, most surprisingly, the actual shape (uniform or Gaussian) of the distribution of colors in the environment.

  12. Molecularly imprinted polymer microspheres prepared by Pickering emulsion polymerization for selective solid-phase extraction of eight bisphenols from human urine samples

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Jiajia [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Li, Yun; Wang, Jincheng [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); Sun, Xiaoli; Cao, Rong [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Sun, Hao [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); Department of Chemistry, Liaoning University, Shenyang 110000 (China); Huang, Chaonan [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Chen, Jiping, E-mail: chenjp@dicp.ac.cn [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China)

    2015-05-04

    Highlights: • BPA imprinted polymer microspheres were prepared by Pickering emulsion polymerization. • Regular spherical shape and narrow diameter distribution. • Good specific adsorption capacity for BPA. • Good class-selectivity and clean-up efficiency for bisphenols in human urine under SPE mode. • Good recoveries and sensitivity for bisphenols using the MIPMS-SPE coupled with HPLC-DAD method. - Abstract: The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption–desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30–60 μm), a specific surface area (S{sub BET}) of 281.26 m{sup 2} g{sup −1} and a total pore volume (V{sub t}) of 0.459 cm{sup 3} g{sup −1}. Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2–2.2 ng mL{sup −1}. The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL{sup −1} for each BP) were in the range of 81.3–106.7% with RSD values below 8.3%.

  13. Form-stable paraffin/high density polyethylene composites as solid-liquid phase change material for thermal energy storage: preparation and thermal properties

    International Nuclear Information System (INIS)

    Sari, Ahmet

    2004-01-01

    This paper deals with the preparation of paraffin/high density polyethylene (HDPE) composites as form-stable, solid-liquid phase change material (PCM) for thermal energy storage and with determination of their thermal properties. In such a composite, the paraffin (P) serves as a latent heat storage material and the HDPE acts as a supporting material, which prevents leakage of the melted paraffin because of providing structural strength. Therefore, it is named form-stable composite PCM. In this study, two kinds of paraffins with melting temperatures of 42-44 deg. C (type P1) and 56-58 deg. C (type P2) and latent heats of 192.8 and 212.4 J g -1 were used. The maximum weight percentage for both paraffin types in the PCM composites without any seepage of the paraffin in the melted state were found as high as 77%. It is observed that the paraffin is dispersed into the network of the solid HDPE by investigation of the structure of the composite PCMs using a scanning electronic microscope (SEM). The melting temperatures and latent heats of the form-stable P1/HDPE and P2/HDPE composite PCMs were determined as 37.8 and 55.7 deg. C, and 147.6 and 162.2 J g -1 , respectively, by the technique of differential scanning calorimetry (DSC). Furthermore, to improve the thermal conductivity of the form-stable P/HDPE composite PCMs, expanded and exfoliated graphite (EG) by heat treatment was added to the samples in the ratio of 3 wt.%. Thereby, the thermal conductivity was increased about 14% for the form-stable P1/HDPE and about 24% for the P2/HDPE composite PCMs. Based on the results, it is concluded that the prepared form-stable P/HDPE blends as composite type PCM have great potential for thermal energy storage applications in terms of their satisfactory thermal properties and improved thermal conductivity. Furthermore, these composite PCMs added with EG can be considered cost effective latent heat storage materials since they do not require encapsulation and extra cost to enhance

  14. Preparation of alumina-coated magnetite nanoparticle for extraction of trimethoprim from environmental water samples based on mixed hemimicelles solid-phase extraction.

    Science.gov (United States)

    Sun, Lei; Zhang, Chuanzhou; Chen, Ligang; Liu, Jun; Jin, Haiyan; Xu, Haoyan; Ding, Lan

    2009-04-13

    In this study, a new type of alumina-coated magnetite nanoparticles (Fe(3)O(4)/Al(2)O(3) NPs) modified by the surfactant sodium dodecyl sulfate (SDS) has been successfully synthesized and applied for extraction of trimethoprim (TMP) from environmental water samples based on mixed hemimicelles solid-phase extraction (MHSPE). The coating of alumina on Fe(3)O(4) NPs not only avoids the dissolving of Fe(3)O(4) NPs in acidic solution, but also extends their application without sacrificing their unique magnetization characteristics. Due to the high surface area of these new sorbents and the excellent adsorption capacity after surface modification by SDS, satisfactory concentration factor and extraction recoveries can be produced with only 0.1g Fe(3)O(4)/Al(2)O(3) NPs. Main factors affecting the adsolubilization of TMP such as the amount of SDS, pH value, standing time, desorption solvent and maximal extraction volume were optimized. Under the selected conditions, TMP could be quantitatively extracted. The recoveries of TMP by analyzing the four spiked water samples were between 67 and 86%, and the relative standard deviation (RSD) ranged from 2 to 6%. Detection and quantification limits of the proposed method were 0.09 and 0.24 microg L(-1), respectively. Concentration factor of 1000 was achieved using this method to extract 500 mL of different environmental water samples. Compared with conventional SPE methods, the advantages of this new Fe(3)O(4)/Al(2)O(3) NPs MHSPE method still include easy preparation and regeneration of sorbents, short times of sample pretreatment, high extraction yields, and high breakthrough volumes. It shows great analytical potential in preconcentration of organic compounds from large volume water samples.

  15. Molecularly imprinted polymer microspheres prepared by Pickering emulsion polymerization for selective solid-phase extraction of eight bisphenols from human urine samples.

    Science.gov (United States)

    Yang, Jiajia; Li, Yun; Wang, Jincheng; Sun, Xiaoli; Cao, Rong; Sun, Hao; Huang, Chaonan; Chen, Jiping

    2015-05-04

    The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption-desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30-60 μm), a specific surface area (S(BET)) of 281.26 m(2) g(-1) and a total pore volume (V(t)) of 0.459 cm(3) g(-1). Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2-2.2 ng mL(-1). The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL(-1) for each BP) were in the range of 81.3-106.7% with RSD values below 8.3%. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Preparation of three-dimensional mesoporous polymer in situ polymerization solid phase microextraction fiber and its application to the determination of seven chlorophenols.

    Science.gov (United States)

    Wang, Xuemei; Wang, Huan; Huang, Pengfei; Ma, Xiaomin; Lu, Xiaoquan; Du, Xinzhen

    2017-01-06

    A superior solid-phase microextraction (SPME) fiber-coating material, three dimensional order mesoporous polymers with Ia-3d bicontinuous cubic structure (3D-OMPs) was in situ coated on a stainless steel wire by solvent evaporation induced self-assembly (EISA) and thermo-polymerization. Fourier-transform infrared spectrometry (FTIR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), small-angel X-ray diffraction (SAXRD), N 2 adsorption-desorption transmission, and thermogravimetry analysis (TGA) were applied to the characterization of the synthesized 3D-OMPs coating. The performance and feasibility of the homemade fiber was evaluated through direct immersion (DI) SPME followed by high-performance liquid chromatography-UV detector (HPLC-UV) for the simultaneous extraction of seven chlorophenols in water samples. Under the optimum conditions, the prepared fiber exhibited excellent extraction properties as compared to three commercial fibers, the DI-SPME-HPLC-UV method showed low limits of detection (0.32-1.85μgL -1 ), wide linear ranges (5.0-1000μgL -1 ), and acceptable reproducibility (relative standard deviation, RSD<7.6% for one fiber, RSD<8.9% for fiber to fiber). Moreover, the method was further successfully applied to the analysis of seven CPs in real samples with good recoveries (80.5-99.5%) and satisfactory precisions (RSD<9.2%). It was confirmed that the proposed method has high sensitivity, outstanding selectivity and good reproducibility to the determination of trace CPs in the environmental water. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. OSMOSE experiment representativity studies.

    Energy Technology Data Exchange (ETDEWEB)

    Aliberti, G.; Klann, R.; Nuclear Engineering Division

    2007-10-10

    The OSMOSE program aims at improving the neutronic predictions of advanced nuclear fuels through measurements in the MINERVE facility at the CEA-Cadarache (France) on samples containing the following separated actinides: Th-232, U-233, U-234, U-235, U-236, U-238, Np-237, Pu-238, Pu-239, Pu-240, Pu-241, Pu-242, Am-241, Am-243, Cm-244 and Cm-245. The goal of the experimental measurements is to produce a database of reactivity-worth measurements in different neutron spectra for the separated heavy nuclides. This database can then be used as a benchmark for integral reactivity-worth measurements to verify and validate reactor analysis codes and integral cross-section values for the isotopes tested. In particular, the OSMOSE experimental program will produce very accurate sample reactivity-worth measurements for a series of actinides in various spectra, from very thermalized to very fast. The objective of the analytical program is to make use of the experimental data to establish deficiencies in the basic nuclear data libraries, identify their origins, and provide guidelines for nuclear data improvements in coordination with international programs. To achieve the proposed goals, seven different neutron spectra can be created in the MINERVE facility: UO2 dissolved in water (representative of over-moderated LWR systems), UO2 matrix in water (representative of LWRs), a mixed oxide fuel matrix, two thermal spectra containing large epithermal components (representative of under-moderated reactors), a moderated fast spectrum (representative of fast reactors which have some slowing down in moderators such as lead-bismuth or sodium), and a very hard spectrum (representative of fast reactors with little moderation from reactor coolant). The different spectra are achieved by changing the experimental lattice within the MINERVE reactor. The experimental lattice is the replaceable central part of MINERVE, which establishes the spectrum at the sample location. This configuration

  18. Representing distance, consuming distance

    DEFF Research Database (Denmark)

    Larsen, Gunvor Riber

    Title: Representing Distance, Consuming Distance Abstract: Distance is a condition for corporeal and virtual mobilities, for desired and actual travel, but yet it has received relatively little attention as a theoretical entity in its own right. Understandings of and assumptions about distance...... are being consumed in the contemporary society, in the same way as places, media, cultures and status are being consumed (Urry 1995, Featherstone 2007). An exploration of distance and its representations through contemporary consumption theory could expose what role distance plays in forming...

  19. Examples of the use of preparative gas-phase chromatography for producing marked molecules; Exemples d'emploi de la chromatographie gazeuse preparative dans la fabrication des molecules marquees

    Energy Technology Data Exchange (ETDEWEB)

    Pichat, L; Baret, Ch; Guermont, J P; Audinot, M [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1960-07-01

    Gas chromatography is most wildly used in the analysis of volatile products. Certain works mention its use for preparatory purposes. Organic labelled molecule preparations are usually made in respect of quantities of the order of 1-10 mmol. It has thus been possible to use gas chromatography with very little alteration for the purification of C-14 labelled molecules and their separation from complex reaction mixtures. The apparatus employed may be briefly described as follows. The chromatography columns used (diameter: 9-12 mm, length: approximately 4-6 m) made it possible to separate labelled products with boiling-points of up to 180 deg. C and in quantities of approximately 100 mg to 1 g. The fractions detected by a conventional conductivity cell device were condensed in traps cooled by liquid nitrogen. The radioactivity was not measured at the same time, as an ionization chamber capable of operating at up to 100 deg. C is still only at the research stage. In all cases, the vector gas was helium and the stationary phase support was usually 80 mesh 'celite 545'. The acetone-2-C{sup 14} produced by pyrolysis of barium acetate was purified on a 'polyglycol 200' column. The water and any unidentified impurities are readily eliminated. The benzene C{sub 6}{sup 14} produced by cyclizing polymerization of the acetylene-C{sup 14} in acetonitril was quantitatively separated from the complex reaction mixture on a nonyl phthalate column at 80 deg. C. The methyl or ethyl acrylates formed, according to Reppe, by the action of radioactive acetylene on a mixture of methanol or ethanol, water an hydrochloric acid, in the presence of nickel carbonyl, are difficult to separate by distillation in small quantities. Two columns were used in series: one consisted of a 'Linde 5 A' molecular sieve having a triple purpose: fixation of the water, fixation of the methanol and neutralization of the hydrochloric acid; the second column composed of nonyl phthalate brought about separation of

  20. Representing AIDS in Comics.

    Science.gov (United States)

    Czerwiec, M K

    2018-02-01

    Matthew P. McAllister wrote: "Comic books can and have contributed positively to the discourse about AIDS: images that encourage true education, understanding and compassion can help cope with a biomedical condition which has more than a biomedical relevance" [1]. With this in mind, I combined a 23-narrator oral history and my personal memoir about an inpatient Chicago AIDS hospital unit in my book, Taking Turns: Stories from HIV/AIDS Care Unit 371. In doing so, I built upon the existing rich history of HIV/AIDS in comics, which this article will briefly describe. Although not a comprehensive review of the intersection of AIDS and comics, the book is a tour through influences that proved useful to me. In addition, in making my book, I faced a distinct ethical issue with regard to representing patient experiences with HIV/AIDS, and I describe here how I addressed it. © 2018 American Medical Association. All Rights Reserved.

  1. Representative of the municipality

    International Nuclear Information System (INIS)

    Castellnou Barcelo, J.

    2007-01-01

    Full text of publication follows. The decommissioning of the Vandellos-I nuclear power plant was a big challenge for the host community of Vandellos i l'Hospitalet de l'Infant and the close-by region. Closing down of the facility resulted in a rise of unemployment and a decrease of municipal income. The public was concerned with three issues: safety, transparency and information about the decommissioning, and economic future. Therefore, from the very beginning, municipal governments entered into negotiations with ENRESA on socio-economic benefits, including local employment in dismantling activities, and other types of financial and non-financial compensation. The ADE business association, i.e. a network of business organisations was created that guided the allotment of work to local firms. To satisfy public demand, local municipalities focused on the triad of safety, dialogue and local development, considered the three 'pillars of trust'. A Municipal Monitoring Commission was created, made up of representatives of affected municipalities, the regional government, the ADE business association, trade unions, the local university, the NPP management and ENRESA to monitor the dismantling process and regularly inform the local public. Items that were handled by this Commission included: - Work process monitoring. - Workers. - Materials Control. - Conventional and radioactive or contaminated waste management. - Emanation waste management (liquid and gas) - Safety (training and accidents). - Surveillance (radiological and environmental: dust, noise). - Effects. - Fulfillment of agreed conditions. A number of communication tools and channels were used, e.g., public information meetings, an information centre, the municipal magazine, the municipal radio station, and meetings with representatives of the local press. Particularly innovative was the idea to ask academics from the University of Tarragona to help with 'translating' technical information into language that could

  2. Preparation of molecularly imprinted solid-phase microextraction fiber for the selective removal and extraction of the antiviral drug abacavir in environmental and biological matrices

    International Nuclear Information System (INIS)

    Terzopoulou, Zoi; Papageorgiou, Myrsini; Kyzas, George Z.; Bikiaris, Dimitrios N.; Lambropoulou, Dimitra A.

    2016-01-01

    In the present study, a molecularly imprinted solid-phase microextraction fiber (MIP-SPME_f) was synthesized and applied for the selective removal and extraction of the antiviral drug, abacavir (ABA). Morphology and structure characterization of fibers were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The effects on the adsorption behavior of the process parameters were studied and the equilibrium data were fitted by the Langmuir, Freundlich and Langmuir-Freundlich models. The maximum adsorption capability (Q_m_a_x) was determined by Langmuir- Freundlich model and was 149 mg/g for MIP-SPME_f. In the next step, SPME methodology followed by liquid desorption and liquid chromatography with mass spectrometry (LC/MS) has been developed and evaluated for the determination of the target compound in environmental and biological matrices (surface waters, wastewaters and urine). Parameters that could influence SPME efficiency were investigated. Then, optimization of stirring speed, extraction time and salt content was carried out by using a central composite design (CCD) and response surface methodology (RSM). A quadratic model between dependent and independent variables was built. Under the optimum conditions (extraction time 40 min, stirring rate 650 rpm and salt content 0.3% NaCl w/v) the validated method presented a high sensitivity and selectivity with LODs and LOQs in the range of 10.1–13.6 and 33.3–43.9 ng/L, respectively. The developed method was successfully applied to the analysis of ABA in real samples. The percentage extraction efficiency ranged from 88 to 99% revealing good accuracy and absence of matrix effects. - Highlights: • Preparation of a novel SPME MIP fiber with remarkable recognition properties. • Selective removal and extraction of abacavir from environmental & biological media. • Detailed adsorbent characterization and adsorption studies. • Successful application of synthesized MIPs

  3. Preparation of molecularly imprinted solid-phase microextraction fiber for the selective removal and extraction of the antiviral drug abacavir in environmental and biological matrices

    Energy Technology Data Exchange (ETDEWEB)

    Terzopoulou, Zoi [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki (Greece); Papageorgiou, Myrsini [Laboratory of Environmental Pollution Control, Department of Chemistry, Aristotle University of Thessaloniki, GR–541 24, Thessaloniki (Greece); Kyzas, George Z.; Bikiaris, Dimitrios N. [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki (Greece); Lambropoulou, Dimitra A., E-mail: dlambro@chem.auth.gr [Laboratory of Environmental Pollution Control, Department of Chemistry, Aristotle University of Thessaloniki, GR–541 24, Thessaloniki (Greece)

    2016-03-24

    In the present study, a molecularly imprinted solid-phase microextraction fiber (MIP-SPME{sub f}) was synthesized and applied for the selective removal and extraction of the antiviral drug, abacavir (ABA). Morphology and structure characterization of fibers were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The effects on the adsorption behavior of the process parameters were studied and the equilibrium data were fitted by the Langmuir, Freundlich and Langmuir-Freundlich models. The maximum adsorption capability (Q{sub max}) was determined by Langmuir- Freundlich model and was 149 mg/g for MIP-SPME{sub f}. In the next step, SPME methodology followed by liquid desorption and liquid chromatography with mass spectrometry (LC/MS) has been developed and evaluated for the determination of the target compound in environmental and biological matrices (surface waters, wastewaters and urine). Parameters that could influence SPME efficiency were investigated. Then, optimization of stirring speed, extraction time and salt content was carried out by using a central composite design (CCD) and response surface methodology (RSM). A quadratic model between dependent and independent variables was built. Under the optimum conditions (extraction time 40 min, stirring rate 650 rpm and salt content 0.3% NaCl w/v) the validated method presented a high sensitivity and selectivity with LODs and LOQs in the range of 10.1–13.6 and 33.3–43.9 ng/L, respectively. The developed method was successfully applied to the analysis of ABA in real samples. The percentage extraction efficiency ranged from 88 to 99% revealing good accuracy and absence of matrix effects. - Highlights: • Preparation of a novel SPME MIP fiber with remarkable recognition properties. • Selective removal and extraction of abacavir from environmental & biological media. • Detailed adsorbent characterization and adsorption studies. • Successful application of

  4. Study on the technical parameters of two different systems of RIA performed with solid-phase antibody test tubes prepared with magnetic microparticle covalence conjagation or conventional physical absorption

    International Nuclear Information System (INIS)

    Chen Zhiqiang; Wang Chengmin; Tang Baojun

    2007-01-01

    Objective: To investigate a new method of preparation of solid-phase antibody with flurorescein isothioeynate (FITC)-anti FITC magnetic nanoparticles system (for FT 3 and TSH). Methods: FT 3 and TSH monoclonal antibody IgC was la- belied with FITC. Anti-FITC magnetic mieroparticles was prepared and conjugated with the FITC labelled antibody to form the solid - phase coated test tube for RIA. Solid-phase test tube prepared with the conventional physical absorption method was also used for RIA and the technical parameters of the two systems were compared. Results: For FT 3 , the sensitivity was 0.18pmol/L with the new method and 0.43pmol/L with the conventional method. Other parameters were; intra-CV, 8.96% vs 16.26%; inter-CV, 15.25% vs 18.83%, correlation with PR method r=0.9825 vs r=0.9102. For TSH, sensitivity was 0.061 μIU/ml vs 0.04 μ IU/ml, intra- CV, 7.6% vs 6.92%, inter-CV, 8.55% vs 14.23%, correlation between the new and conventional method, r=0. 9987. TSH RIA was especially rapid with the new technic: 79 min vs 190 min. Conclusion: For FT 3 and TSH RIA, the new method takes much less time with increased homogeniety. (authors)

  5. Pressure-driven one-step solid phase-based on-chip sample preparation on a microfabricated plastic device and integration with flow-through polymerase chain reaction (PCR).

    Science.gov (United States)

    Tran, Hong Hanh; Trinh, Kieu The Loan; Lee, Nae Yoon

    2013-10-01

    In this study, we fabricate a monolithic poly(methylmethacrylate) (PMMA) microdevice on which solid phase-based DNA preparation and flow-through polymerase chain reaction (PCR) units were functionally integrated for one-step sample preparation and amplification operated by pressure. Chelex resin, which is used as a solid support for DNA preparation, can capture denatured proteins but releases DNA, and the purified DNA can then be used as a template in a subsequent amplification process. Using the PMMA microdevices, DNA was successfully purified from both Escherichia coli and human hair sample, and the plasmid vector inserted in E. coli and the D1S80 locus in human genomic DNA were successfully amplified from on-chip purified E. coli and human hair samples. Furthermore, the integration potential of the proposed sample preparation and flow-through PCR units was successfully demonstrate on a monolithic PMMA microdevice with a seamless flow, which could pave the way for a pressure-driven, simple one-step sample preparation and amplification with greatly decreased manufacture cost and enhanced device disposability. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Verification of Representative Sampling in RI waste

    International Nuclear Information System (INIS)

    Ahn, Hong Joo; Song, Byung Cheul; Sohn, Se Cheul; Song, Kyu Seok; Jee, Kwang Yong; Choi, Kwang Seop

    2009-01-01

    For evaluating the radionuclide inventories for RI wastes, representative sampling is one of the most important parts in the process of radiochemical assay. Sampling to characterized RI waste conditions typically has been based on judgment or convenience sampling of individual or groups. However, it is difficult to get a sample representatively among the numerous drums. In addition, RI waste drums might be classified into heterogeneous wastes because they have a content of cotton, glass, vinyl, gloves, etc. In order to get the representative samples, the sample to be analyzed must be collected from selected every drum. Considering the expense and time of analysis, however, the number of sample has to be minimized. In this study, RI waste drums were classified by the various conditions of the half-life, surface dose, acceptance date, waste form, generator, etc. A sample for radiochemical assay was obtained through mixing samples of each drum. The sample has to be prepared for radiochemical assay and although the sample should be reasonably uniform, it is rare that a completely homogeneous material is received. Every sample is shredded by a 1 ∼ 2 cm 2 diameter and a representative aliquot taken for the required analysis. For verification of representative sampling, classified every group is tested for evaluation of 'selection of representative drum in a group' and 'representative sampling in a drum'

  7. Pharmacokinetics, pharmacodynamics, efficacy, and safety of a new recombinant asparaginase preparation in children with previously untreated acute lymphoblastic leukemia: A randomized phase 2 clinical trial

    NARCIS (Netherlands)

    R. Pieters (Rob); I.M. Appel (Inge); H.J. Kuehnel; I. Tetzlaff-Fohr (Iris); U. Pichlmeier (Uwe); I. van der Vaart (Inekee); E. Visser (Eline); R.L. Stigter

    2008-01-01

    textabstractThe pharmacokinetics, pharmacodynam-ics, efficacy, and safety of a new recom-binant Escherichia coli - asparaginase preparation was compared withAsparagi-nase medac. Thirty-two children with acute lymphoblastic leukemia were randomized to receive one of both agents at a dose of 5000

  8. Immunostimulation in the urinary bladder by local application of Nocardia rubra cell wall skeleton preparation (Rubratin) for superficial bladder cancer immunotherapy--a phase I/II study

    NARCIS (Netherlands)

    de Reijke, T. M.; de Boer, E. C.; Schamhart, D. H.; Kurth, K. H.

    1997-01-01

    Twelve patients with superficial papillary transitional cell carcinoma of the bladder (pTa, pT1) were treated with six consecutive weekly intravesical instillations of Rubratin (in a dose of 1.5, 3.0, or 4.5 mg), a cell wall skeleton preparation of Nocardia rubra (NCW). The main objective of this

  9. Simultaneous determination of 15 marker constituents in various radix Astragali preparations by solid-phase extraction and high-performance liquid chromatography.

    Science.gov (United States)

    Qi, Lian-Wen; Yu, Qing-Tao; Yi, Ling; Ren, Mei-Ting; Wen, Xiao-Dong; Wang, Yu-Xia; Li, Ping

    2008-01-01

    An improved quality control method was developed to simultaneously determine 15 major constituents (eight flavonoids and seven saponins) in various radix Astragali preparations, using SPE for pretreatment of samples, HPLC with diode-array and evaporative light scattering detectors (DAD-ELSD) for quantification in one run, and HPLC-ESI-TOF/MS for definite identification of compounds in preparations. Optimum separations were obtained with a ZORBAX C(18) column, using a gradient elution with 0.3% aqueous formic acid and ACN. This established method was fully validated with respect to linearity, precision, repeatability, and accuracy, and was successfully applied to quantify the 15 compounds in 19 commercial samples, including 3 dosage forms, i. e., oral solution, injection, concentrated granule, and its processed products of radix Astragali. The results demonstrated that many factors might result in significant differences in quality of the final preparations, including crude drugs, pretreatment processes, manufacturing procedure, storage conditions, etc. Then the developed method provided a reasonable and powerful manner to ensure the efficacy, safety, and batch-to-batch uniformity of radix Astragali products by standardizing each procedure, and thus should be proposed as quality control for the clinical use and modernization of herbal preparations.

  10. Preparation of sulfur/multiple pore size porous carbon composite via gas-phase loading method for lithium-sulfur batteries

    International Nuclear Information System (INIS)

    Li, Long-Yan; Chen, Yan-Xiao; Guo, Xiao-Dong; Zhong, Ben-He; Zhong, Yan-Jun

    2014-01-01

    A porous carbon with multiple pore size distribution was synthesized, and regarded as a carrier to obtain the sulfur/carbon (S/C) composite via a gas-phase loading method. We proposed this novel gas-phase loading method by using a specially designed fluid-bed reactor to encapsulate and sequester gas-phase sulfur molecules into the porous carbon in current study. The nitrogen Brunauer-Emmett-Teller (BET), scanning electron microscopy (SEM) and X-ray powder diffraction (XRD) characterizations were investigated on both the porous carbon and the sulfur/carbon composite. The results show that the gas-phase loading method contributes to the combination of sulfur molecules and matrix porous carbon. Furthermore, the sulfur/multiple pore size distribution carbon composite based on the gas-phase loading method demonstrate an excellent electrochemical property. The initial specific discharge capacity is 795.0 mAh g −1 at 800 mA g −1 , with a capacity retention of 86.3% after 100 cycles

  11. Heterogeneous catalysis in liquid-phase oxidation of olefin--2. Dependence of the structure of vanadium-chromium binary oxide catalyst for oxidation of cyclohexene on the method of preparation

    Energy Technology Data Exchange (ETDEWEB)

    Takehira, K; Hayakawa, T; Ishikawa, T

    1978-01-01

    Dependence of the structure of vanadium-chromium binary oxide catalyst for oxidation of cyclohexene on the method of preparation was studied in an extension of previous work by using three series of binary oxide catalysts, D, E, and F, which were prepared by coprecipitation from acidic, neutral, and alkaline media, respectively. The specific activity at 60/sup 0/C, 1 atm oxygen, and benzene solvent decreased in the order D > E > F, but all three series showed maximum activity at 90% chromium. The selectivity for epoxide also followed the order D > E > F, but the maximum selectivity occurred at 50% chromium for D, 75% for E, and 90% for F. Comparison of these results with X-ray diffraction and ESR spectral structural analysis of the various chromium(III) vanadate phases supported the previously proposed mechanism, with cyclohexene autoxidation initiated by free radical decomposition of cyclohexene hydroperoxide occurring on a different type of active site.

  12. Direct crystallization of perovskite phase in PMN-PT thin films prepared by polyvinylpyrrolidone modified sol-gel processing and their properties

    International Nuclear Information System (INIS)

    Du, Z.H.; Zhang, T.S.; Zhu, M.M.; Ma, J.

    2009-01-01

    A modified sol-gel processing has been developed by using polyvinylpyrrolidone (PVP) as modifier and lead nitrate as lead source to synthesize (1-x)Pb(Mg 1/3 ,Nb 2/3 )O 3 -xPbTiO 3 (PMN-PT) thin films with x=0.23-0.43. With PVP additions, perovskite phase could directly crystallize from amorphous films at the temperature as low as 430 deg. C via bypassing the metastable phase-pyrochlore and crystallinity was significantly enhanced. The PVP addictives have been optimized with molecular weight 1/3 ,Nb 2/3 )O 3 -PbTiO 3 films via bypassing pyrochlore phase.

  13. Phase-inversion tape-casting preparation and significant performance enhancement of Ce0.9Gd0.1O1.95- La0.6Sr0.4Co0.2Fe0.8O3-δ dual-phase asymmetric membrane for oxygen separation

    DEFF Research Database (Denmark)

    Huang, Hua; Cheng, Shiyang; Gao, Jianfeng

    2014-01-01

    The dual-phase Ce0.9Gd0.1O1.95–La0.6Sr0.4Co0.2Fe0.8O3−δ asymmetric membrane was prepared via a phase-inversion tape-casting method. The membrane consisted of a thicker porous support layer and a thinner dense layer. When the dense side of the membrane was coated with a La0.6Sr0.4CoO3−δ catalytic...

  14. Mechanisms of membrane protein insertion into liposomes during reconstitution procedures involving the use of detergents. 1. Solubilization of large unilamellar liposomes (Prepared by reverse-phase evaporation) by Triton X-100 octyl glucoside, and sodium cholate

    International Nuclear Information System (INIS)

    Paternostre, M.T.; Roux, M.; Rigaud, J.L.

    1988-01-01

    The mechanisms governing the solubilization by Triton X-100, octyl glucoside, and sodium cholate of large unilamellar liposomes prepared by reverse-phase evaporation were investigated. The solubilization process is described by the three-stage model previously proposed for the detergents. In stage I, detergent monomers are incorporated into the phospholipid bilayers until they saturate the liposomes. At this point, i.e., stage II, mixed phospholipid-detergent micelles begin to form. By stage III, the lamellar to micellar transition is complete and all the phospholipids are present as mixed micelles. The turbidity of liposome preparations was systematically measured as a function of the amount of detergent added for a wide range of phospholipid concentrations. The results allowed a quantitative determination of the effective detergent to lipid molar ratios in the saturated liposomes. The monomer concentrations of the three detergents in the aqueous phase were also determined at the lamellar to micellar transitions. These transitions were also investigated by 31 P NMR spectroscopy, and complete agreement was found with turbidity measurements. Freeze-fracture electron microscopy and permeability studies in the sublytic range of detergent concentrations indicated that during stage I of solubilization detergent partitioning between the aqueous phase and the lipid bilayer greatly affects the basic permeability of the liposomes without significantly changing the morphology of the preparations. A rough approximation of the partition coefficients was derived from the turbidity and permeability data. It is concluded that when performed systematically, turbidity measurements constitute a very convenient and powerful technique for the quantitative study of the liposome solubilization process by detergents

  15. MC3T3-E1 cell response of amorphous phase/TiO{sub 2} nanocrystal composite coating prepared by microarc oxidation on titanium

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Rui [Department of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Wei, Daqing, E-mail: daqingwei@hit.edu.cn [Department of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Yang, Haoyue; Feng, Wei [Department of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Cheng, Su [Department of Mechanical Engineering, School of Architecture and Civil Engineering, Harbin University of Science and Technology, Harbin 150001 (China); Li, Baoqiang; Wang, Yaming; Jia, Dechang; Zhou, Yu [Department of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China)

    2014-06-01

    Bioactive amorphous phase/TiO{sub 2} nanocrystal (APTN) composite coatings were fabricated by microarc oxidation (MAO) on Ti. The APTN coatings are composed of much amorphous phase with Si, Na, Ca, Ti and O elements and a few TiO{sub 2} nanocrystals. With increasing applied voltage, the micropore density of the APTN coating decreases and the micropore size of the APTN coating increases. The results indicate that less MC3T3-E1 cells attach on the APTN coatings as compared to Ti. However, the APTN coatings greatly enhance the cell proliferation ability and the activity of alkaline phosphatase. The amorphous phase and the concentrations of the released Ca and Si from the APTN coatings during cell culture have significant effects on the cell response. - Highlights: • Amorphous phase/TiO2 nanocrystal (APTN) composite coatings were fabricated. • The MC3T3-E1 cell response of the APTN coatings was evaluated. • The APTN coatings greatly enhanced the cell proliferation ability.

  16. Measurement of the quantum superposition state of an imaging ensemble of photons prepared in orbital angular momentum states using a phase-diversity method

    International Nuclear Information System (INIS)

    Uribe-Patarroyo, Nestor; Alvarez-Herrero, Alberto; Belenguer, Tomas

    2010-01-01

    We propose the use of a phase-diversity technique to estimate the orbital angular momentum (OAM) superposition state of an ensemble of photons that passes through an optical system, proceeding from an extended object. The phase-diversity technique permits the estimation of the optical transfer function (OTF) of an imaging optical system. As the OTF is derived directly from the wave-front characteristics of the observed light, we redefine the phase-diversity technique in terms of a superposition of OAM states. We test this new technique experimentally and find coherent results among different tests, which gives us confidence in the estimation of the photon ensemble state. We find that this technique not only allows us to estimate the square of the amplitude of each OAM state, but also the relative phases among all states, thus providing complete information about the quantum state of the photons. This technique could be used to measure the OAM spectrum of extended objects in astronomy or in an optical communication scheme using OAM states. In this sense, the use of extended images could lead to new techniques in which the communication is further multiplexed along the field.

  17. High-temperature oxidation of silicide-aluminide layer on the TiAl6V4 alloy prepared by liquid-phase siliconizing

    Czech Academy of Sciences Publication Activity Database

    Kubatík, Tomáš František

    2016-01-01

    Roč. 50, č. 2 (2016), s. 257-261 ISSN 1580-2949 Institutional support: RVO:61389021 Keywords : TiAl6V4 * silicides * high-temperature oxidation * liquid-phase silicon izing Subject RIV: JG - Metallurgy Impact factor: 0.436, year: 2016

  18. A Lab on a chip device for rapid identification of Avian Influenza virus by on-chip sample preparation and solid phase PCR

    DEFF Research Database (Denmark)

    Yi, Sun; Dhumpa, Raghuram; Bang, Dang Duong

    2009-01-01

    In this paper, we describe a novel lab-on-a-chip device for fast AIV screening by integrating DNA microarray-based solid phase PCR on microchip. The device can handle viral samples in an automatic way. Moreover, multiplex PCR and sequence detection are done in one-step, which greatly simplifies...

  19. Preparation of detergent-lipase complexes utilizing water-soluble amphiphiles in single aqueous phase and catalysis of transesterifications in homogeneous organic solvents.

    Science.gov (United States)

    Mine, Y; Fukunaga, K; Maruoka, N; Nakao, K; Sugimura, Y

    2000-01-01

    A novel method of preparing detergent-enzyme complexes that can be employed in organic media was developed utilizing newly synthesized water-soluble nonionic gemini-type detergents, N,N-bis(3-D-gluconamidopropyl)-3-(dialkyl-L-glutamatecarbonyl)propanamides (BIG2CnCA: n = 10,12,14,16,18) and N,N-bis(3-D-lactonamidopropyl)-3-(dialkyl-L-glutamatecarbonyl)propanamides (BIL2CnCA: n = 16,18), and nonionic twin-headed detergents, N,N-bis(3-D-gluconamidopropyl)alkanamides (BIG1Cn: n = 12,14,16,18,delta9). This method simply entails mixing a selected enzyme with an appropriate detergent in an aqueous solution followed by lyophilization, and it offers the advantages of enhanced enzymatic activity in organic solvents and eliminates both enzyme loss and the necessity for an organic solvent in the preparation stage. Using various modified lipases originating from Aspergillus niger (Lipase A), Candida rugosa (Lipase C), Pseudomonas cepacia (Lipase P), and porcine pancreas (PPL), prepared using the novel method and detergents, including conventional synthesized nonionic detergents such as dialkyl N-D-glucona-L-glutamates (2CnGE: n = 12,18delta9) and octanoyl-N-methylglucamide (MEGA-8), enantioselective transesterifications of 6-methyl-5-hepten-2-ol (sulcatol) and 2,2-dimethyl-1,3-dioxolane-4-methanol (solketal) with a vinyl or isopropenyl carboxylate were carried out in an organic solvent. The modified lipase activity was influenced by both the lipases and the structure of the detergents. The value for the hydrophile-lipophile balance (HLB) of the detergent provided a means of correlating the structure and the obtained modified lipase activity. For detergents of the same class with a HLB value of approximately 9 and 12, the highest activity was obtained for Lipase A and Lipase P, and Lipase C and PPL, respectively. Among detergents of the same HLB value tested, the gemini-type detergents possessing the most bulky head and tail were most effective as a modifier for lipases of all

  20. Low Thermal Conductivity of RE-Doped SrO(SrTiO3)1 Ruddlesden Popper Phase Bulk Materials Prepared by Molten Salt Method

    Science.gov (United States)

    Putri, Yulia Eka; Said, Suhana Mohd; Refinel, Refinel; Ohtaki, Michitaka; Syukri, Syukri

    2018-04-01

    The SrO(SrTiO3)1 (Sr2TiO4) Ruddlesden Popper (RP) phase is a natural superlattice comprising of alternately stacking perovskite-type SrTiO3 layers and rock salt SrO layers along the crystallographic c direction. This paper discusses the properties of the Sr2TiO4 and (La, Sm)-doped Sr2TiO4 RP phase synthesized via molten salt method, within the context of thermoelectric applications. A good thermoelectric material requires high electrical conductivity, high Seebeck coefficient and low thermal conductivity. All three conditions have the potential to be fulfilled by the Sr2TiO4 RP phase, in particular, the superlattice structure allows a higher degree of phonon scattering hence resulting in lowered thermal conductivity. In this work, the Sr2TiO4 RP phase is doped with Sm and La respectively, which allows injection of charge carriers, modification of its electronic structure for improvement of the Seebeck coefficient, and most significantly, reduction of thermal conductivity. The particles with submicron size allows excessive phonon scattering along the boundaries, thus reduces the thermal conductivity by fourfold. In particular, the Sm-doped sample exhibited even lower lattice thermal conductivity, which is believed to be due to the mismatch in the ionic radius of Sr and Sm. This finding is useful as a strategy to reduce thermal conductivity of Sr2TiO4 RP phase materials as thermoelectric candidates, by employing dopants of differing ionic radius.

  1. Preparation and quantification of the total phenolic products in Citrus fruit using solid-phase extraction coupled with high-performance liquid chromatography with diode array and UV detection.

    Science.gov (United States)

    Zeng, Honglian; Liu, Zhenli; Zhao, Siyu; Shu, Yisong; Song, Zhiqian; Wang, Chun; Dong, Yunzhuo; Ning, Zhangchi; He, Dan; Wang, Menglei; Lu, Cheng; Liu, Yuanyan; Lu, Aiping

    2016-10-01

    Citrus fruit is an important health-promoting food that is rich in dietary phenolic metabolites. Traditional Chinese medicines, such as Zhishi and Zhiqiao, come from young and immature fruits of Citrus cultivars. The preparation of diversified bioactive phenolic products and establishment of the corresponding quality control methodology are challenging and necessary. In the current study, four types of solid-phase extraction sorbents for the enrichment and clean-up of the phenolic matrix were evaluated. A solid-phase extraction column coated with Strata-X was finally used in the procedure. Twenty phenolic compounds were selected to evaluate the extraction performances of the sorbents using high-performance liquid chromatography analysis. Under the optimized conditions, good linearities were obtained with R 2 more than 0.9996 for all analytes with LODs of 0.04-1.012 μg/g. Intra- and interday relative standard deviation values were less than 3%, and the recovery was equal to or higher than 90.02%. Compared to non-solid-phase extraction process, the content of total phenolic products was elevated 35.55-68.48% with solid-phase extraction. Finally, the developed and validated method was successfully applied to the discrimination of Zhishi samples from different species as well as Zhishi and Zhiqiao samples in different development stages. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Crystallite-growth, phase transition, magnetic properties, and sintering behaviour of nano-CuFe2O4 powders prepared by a combustion-like process

    International Nuclear Information System (INIS)

    Köferstein, Roberto; Walther, Till; Hesse, Dietrich; Ebbinghaus, Stefan G.

    2014-01-01

    The synthesis of nano-crystalline CuFe 2 O 4 powders by a combustion-like process is described herein. Phase formation and evolution of the crystallite size during the decomposition process of a (CuFe 2 )—precursor gel were monitored up to 1000 °C. Phase-pure nano-sized CuFe 2 O 4 powders were obtained after reaction at 750 °C for 2 h resulting in a crystallite size of 36 nm, which increases to 96 nm after calcining at 1000 °C. The activation energy of the crystallite growth process was calculated as 389 kJ mol −1 . The tetragonal⇄cubic phase transition occurs between 402 and 419 °C and the enthalpy change (ΔH) was found to range between 1020 and 1229 J mol −1 depending on the calcination temperature. The optical band gap depends on the calcination temperature and was found between 2.03 and 1.89 eV. The shrinkage and sintering behaviour of compacted powders were examined. Dense ceramic bodies can be obtained either after conventional sintering at 950 °C or after a two-step sintering process at 800 °C. Magnetic measurements of both powders and corresponding ceramic bodies show that the saturation magnetization rises with increasing calcination-/sintering temperature up to 49.1 emu g −1 (2.1 µ B fu −1 ), whereas the coercivity and remanence values decrease. - Graphical abstract: A cheap one-pot synthesis was developed to obtain CuFe 2 O 4 nano-powders with different crystallite sizes (36–96 nm). The optical band gaps, phase transition temperatures and enthalpies were determined depending on the particle size. The sintering behaviour of nano CuFe 2 O 4 was studied in different sintering procedures. The magnetic behaviour of the nano-powders as well as the corresponding ceramic bodies were investigated. - Highlights: • Eco-friendly and simple synthesis for nano CuFe 2 O 4 powder using starch as polymerization agent. • Monitoring the phase evolution and crystallite growth kinetics during the synthesis. • Determination of the optical band gap

  3. TiO{sub 2} based photo-catalysts prepared by chemical vapor infiltration (CVI) on micro-fibrous substrates; Photocatalyseurs a base de TiO{sub 2} prepares par infiltration chimique en phase vapeur (CVI) sur supports microfibreux

    Energy Technology Data Exchange (ETDEWEB)

    Sarantopoulos, Ch

    2007-10-15

    This thesis deals with micro-fibrous glass substrates functionalized with TiO{sub 2}. The oxide is deposited as a thin film onto the micro fibres by chemical vapour infiltration (CVI), yielding a photo-catalytic material usable for cleaning polluted air. We studied the relation between the structure of the material and its photo-catalytic efficiency. TiO{sub 2} thin films were prepared at low pressure, in a hot-wall CVD reactor, using Ti(O-iPr){sub 4} as a precursor. They were characterized by XRD, SEM, EDX, XPS and BET, and by recording the kinetics of decomposition of varied pollutants in solution (orange G, malic acid, imazapyr) and in air (toluene). The conditions favoring the growth of porous films through a columnar growth mode were established by MOCVD-depositing TiO{sub 2} thin films on flat substrates. The subsequent works with micro fibrous thick substrates showed the uniformity of infiltration to be the main factor governing the photo-catalytic efficiency. Operating parameters that optimize infiltration do not yield columnar growth mode. A compromise is necessary. Our photo-catalysts are showing high efficiency comparable, if not higher, to those actually commercialized. These promising results are opening real perspectives for the proposed process. (author)

  4. Advanced fluidic handling and use of two-phase flow for high throughput structural investigation of proteins on a microfluidic sample preparation platform

    DEFF Research Database (Denmark)

    Lafleur, Josiane P.; Snakenborg, Detlef; Møller, M.

    2010-01-01

    Research on the structure of proteins can bring forth a wealth of information about biological function and can be used to better understand the processes in living cells. This paper reports a new microfluidic sample preparation system for the structural investigation of proteins by Small Angle X......-ray Scattering (SAXS). The system includes hardware and software features for precise fluidic control, synchrotron beamline control, UV absorbance measurements and automated data analysis. The precise fluidic handling capabilities are used to transport and precisely position samples as small as 500 n...

  5. The use of solid phase microextraction as sample preparation technique for determination of n-nitrosodimethylamine in water polluted by hydrazine-based rocket fuel

    Directory of Open Access Journals (Sweden)

    Bulat Kenessov

    2009-05-01

    Full Text Available A paper describes a method for determination of N-nitrosodimethylamine in water, polluted by spills of 1,1-dimethylhydrazine, based on solid phase microextraction coupled to gas chromatography/mass spectrometry. A method detection limit was determined to be 1 ug/kg, relative error was below 20%. A method is very sensitive and selective as well as quite simple, relatively cheap and fully automated.

  6. Preparation and characterization of sodium dodecyl sulfate doped polypyrrole solid phase micro extraction fiber and its application to endocrine disruptor pesticide analysis

    OpenAIRE

    Korba, Korcan; Pelit, Levent; Okçu Pelit, Füsun; Özdokur, K. Volkan; Ertaş, Hasan; Eroğlu, Ahmet E.; Ertaş, Fatma Nil

    2013-01-01

    A robust in house solid-phase micro extraction (SPME) surface has been developed for the headspace (HS)-SPME determination of endocrine disruptor pesticides, namely, Chlorpyrifos, Penconazole, Procymidone, Bromopropylate and Lambda-Cyhalothrin in wine sample by using sodium dodecylsulfate doped polypyrrole SPME fiber. Pyrrole monomer was electrochemically polymerized on a stainless steel wire in laboratory conditions in virtue of diminishing the cost and enhancing the analyte retention on its...

  7. Facile preparation of multifunctional carbon nanotube/magnetite/polyaniline nanocomposite offering a strong option for efficient solid-phase microextraction coupled with GC-MS for the analysis of phenolic compounds.

    Science.gov (United States)

    Tafazoli, Zahra; Azar, Parviz Aberoomand; Tehrani, Mohammad Saber; Husain, Syed Waqif

    2018-04-20

    The aim of this study the synthesis of a highly efficient organic-inorganic nanocomposite. In this research, the carbon nanotube/magnetite/polyaniline nanocomposite was successfully prepared through a facile route. Monodisperse magnetite nanospheres were prepared through the coprecipitation route, and polyaniline nanolayer as a modified shell with a high surface area was synthesized by an in situ growth route and characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and energy dispersive X-ray spectroscopy. The prepared nanocomposite was immobilized on a stainless-steel wire for the fabrication of the solid-phase microextraction fiber. The combination of headspace solid-phase microextraction using carbon nanotube/magnetite/polyaniline nanocomposite fiber with gas chromatography and mass spectrometry can achieve a low limit of detection and can be applied to determine phenolic compounds in water samples. The effects of the extraction and desorption parameters including extraction temperature and time, ionic strength, stirring rate, pH, and desorption temperature and time have been studied. Under the optimum conditions, the dynamic linear range was 0.01-500 ng mL -1 and the limits of detection of phenol, 4-chlorophenol, 2,6-dichlorophenol, and 2,4,6-trichlorophenol were the lowest (0.008 ng mL -1 ) for three times. The coefficient of determination of all calibration curves was more than 0.990. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  8. Preparation of tazheranite powders by solid phase reaction and conductivity of sintered bodies. Kosoho ni yoru tazheranite no funmatsu gosei to dodensei

    Energy Technology Data Exchange (ETDEWEB)

    Kuramochi, H; Kobayashi, H; Mitamura, T [Saitama University, Saitama (Japan). Faculty of Enginering; Mori, T; Yamamura, H [Tosoh Co., Tokyo (Japan)

    1992-09-01

    Single phase powder of Ca0.2Zr(0.8-x)TixOy was synthesized by replacing a part of ZrO2 in tazheranite which belongs to cubic crystal mineral of 3 constituents of CaO/ZrO2/ TiO2 with TiO2 to study the conductivity. Predetermined powder amounts of CaCO3, ZrO2 and TiO2 were respectively weighed and mixed with wet condition, the carbonate was decomposed at 1,000 centigrade, and after mixed again with wet condition, the mixture was dried and calcined again at 1,200 to 1,300 centigrade for 2 to 20 hours to get the powder. This powder was crushed and classified to make molded items by uniaxial pressing and the items were fired at 1,400 to 1,600 centigrade for 1 to 10 hours. The conductivity of sintered bodies was measured by the complex impedance method. The following results could be obtained: The targeted powder could be synthesized at the composition range of x=0.04 to 0.10 and the apparent x of single phase area was widened to 0.15 at the firing temperature of 1,500 centigrade. The activation energies of the conductivity of sintered items were 120 to 130kJ/mol, indicating that the electric conductivity was dominated by the ion conduction and was not affected by TiO2 amount, and the formed phase. The grain resistance increased and the grain boundary resistance decreased with the increase of TiO2 amount. 17 refs., 9 figs.

  9. Solid phase reduction of 99mTcO4radical with zinc: a method for the preparation of difficult 99mTc complexes

    International Nuclear Information System (INIS)

    Kremer, C.; Leon, A.; Gambino, D.; Cartesio, S.; Ures, C.; Savio, E.; Campos, E.; Kremer, E.

    1989-01-01

    Two groups of compounds: aminoacids (glutamic acid, glutamine, glycine, lysine) and amines (ethylenediamine, diethylenetriamine, o-phenantroline, o-phenylenediamine) have been labelled with 99m Tc by means of a solid phase reduction using fine powdered zinc as reducing agent. In all cases radiochemical purity in excess of 90% was obtained, with no evidence of colloid formation. Labelling yields were variable depending on the ligand used. The results show that the method presented allows labelling some molecules with 99m Tc for which the use of conventional techniques are not feasible. (author)

  10. Preparation of macroporous zirconia monoliths from ionic precursors via an epoxide-mediated sol-gel process accompanied by phase separation

    International Nuclear Information System (INIS)

    Guo, Xingzhong; Song, Jie; Lvlin, Yixiu; Yang, Hui; Nakanishi, Kazuki; Kanamori, Kazuyoshi

    2015-01-01

    Monolithic macroporous zirconia (ZrO 2 ) derived from ionic precursors has been successfully fabricated via the epoxide-mediated sol-gel route accompanied by phase separation in the presence of propylene oxide (PO) and poly(ethylene oxide) (PEO). The addition of PO used as an acid scavenger mediates the gelation, whereas PEO enhances the polymerization-induced phase separation. The appropriate choice of the starting compositions allows the production of a macroporous zirconia monolith with a porosity of 52.9% and a Brunauer–Emmett–Teller (BET) surface area of 171.9 m 2 · g −1 . The resultant dried gel is amorphous, whereas tetragonal ZrO 2 and monoclinic ZrO 2 are precipitated at 400 and 600 °C, respectively, without spoiling the macroporous morphology. After solvothermal treatment with an ethanol solution of ammonia, tetragonal ZrO 2 monoliths with smooth skeletons and well-defined mesopores can be obtained, and the BET surface area is enhanced to 583.8 m 2 · g −1 . (paper)

  11. Role of phase composition for electronic states in CH{sub 3}NH{sub 3}PbI{sub 3} prepared from CH{sub 3}NH{sub 3}I/PbCl{sub 2} solution

    Energy Technology Data Exchange (ETDEWEB)

    Naikaew, Atittaya; Prajongtat, Pongthep [Helmholtz-Center Berlin for Energy and Materials, Institute of Heterogeneous Materials, Hahn-Meitner-Platz 1, D-14109 Berlin (Germany); Department of Materials Science, Faculty of Science, Kasetsart University, Bangkok 10900 (Thailand); Lux-Steiner, Martha Ch.; Dittrich, Thomas, E-mail: dittrich@helmholtz-berlin.de [Helmholtz-Center Berlin for Energy and Materials, Institute of Heterogeneous Materials, Hahn-Meitner-Platz 1, D-14109 Berlin (Germany); Arunchaiya, Marisa [Department of Materials Science, Faculty of Science, Kasetsart University, Bangkok 10900 (Thailand)

    2015-06-08

    Modulated surface photovoltage (SPV) spectra have been correlated with the phase composition in layers of CH{sub 3}NH{sub 3}PbI{sub 3} (MAPbI{sub 3}) prepared from MAI and PbCl{sub 2} and annealed at 100 °C. Depending on the annealing time, different compositions of MAPbI{sub 3}, MAPbCl{sub 3}, MACl, PbI{sub 2}, and an un-identified phase were found. It has been demonstrated that evaporation of MAI and HI is crucial for the development of electronic states in MAPbI{sub 3} and that only the appearance and evolution of the phase PbI{sub 2} has an influence on electronic states in MAPbI{sub 3}. With ongoing annealing, (i) a transition from p- to n-type doping was observed with the appearance of PbI{sub 2}, (ii) shallow acceptor states were distinguished and disappeared in n-type doped MAPbI{sub 3}, and (iii) a minimum of the SPV response related to deep defect states was found at the transition from p- to n-type doping. The results are discussed with respect to the further development of highly efficient and stable MAPbI{sub 3} absorbers for solar cells.

  12. Effects of meal preparation training on body weight, glycemia, and blood pressure: results of a phase 2 trial in type 2 diabetes

    Directory of Open Access Journals (Sweden)

    Dasgupta Kaberi

    2012-10-01

    Full Text Available Abstract Background Modest reductions in weight and small increases in step- related activity (e.g., walking can improve glycemic and blood pressure control in type 2 diabetes mellitus (DM2. We examined changes in these parameters following training in time- efficient preparation of balanced, low- energy meals combined with pedometer- based step count monitoring. Methods Seventy- two adults with DM2 were enrolled in a 24- week program (i.e., 15 three- hour group sessions. They prepared meals under a chef’s supervision, and discussed eating behaviours/nutrition with a registered dietitian. They maintained a record of pedometer- assessed step counts. We evaluated changes from baseline to 24 weeks in terms of weight, step counts, hemoglobin A1c (HbA1c, glycemic control, blood pressure, and eating control ability (Weight Efficacy Lifestyle WEL Questionnaire. 53 participants (73.6% completed assessments. Results There were improvements in eating control (11.2 point WEL score change, 95% CI 4.7 to 17.8, step counts (mean change 869 steps/day, 95% CI 198 to 1,540, weight (mean change −2.2%; 95% CI −3.6 to −0.8, and HbA1c (mean change −0.3% HbA1c, 95% CI −0.6 to −0.1, as well as suggestion of systolic blood pressure reduction (mean change −3.5 mm Hg, 95% CI −7.8 to 0.9. Findings were not attributable to medication changes. In linear regression models (adjusted for age, sex, ethnicity, insulin use, season, a −2.5% weight change was associated with a −0.3% HbA1c change (95% CI −0.4 to −0.2 and a −3.5% systolic blood pressure change (95% CI −5.5 to −1.4. Conclusions In this ‘proof of concept’ study, persistence with the program led to improvements in eating and physical activity habits, glycemia reductions, and suggestion of blood pressure lowering effects. The strategy thus merits further study and development to expand the range of options for vascular risk reduction in DM2.

  13. Effects of meal preparation training on body weight, glycemia, and blood pressure: results of a phase 2 trial in type 2 diabetes.

    Science.gov (United States)

    Dasgupta, Kaberi; Hajna, Samantha; Joseph, Lawrence; Da Costa, Deborah; Christopoulos, Stavroula; Gougeon, Rejeanne

    2012-10-17

    Modest reductions in weight and small increases in step- related activity (e.g., walking) can improve glycemic and blood pressure control in type 2 diabetes mellitus (DM2). We examined changes in these parameters following training in time- efficient preparation of balanced, low- energy meals combined with pedometer- based step count monitoring. Seventy- two adults with DM2 were enrolled in a 24- week program (i.e., 15 three- hour group sessions). They prepared meals under a chef's supervision, and discussed eating behaviours/nutrition with a registered dietitian. They maintained a record of pedometer- assessed step counts. We evaluated changes from baseline to 24 weeks in terms of weight, step counts, hemoglobin A1c (HbA1c, glycemic control), blood pressure, and eating control ability (Weight Efficacy Lifestyle WEL Questionnaire). 53 participants (73.6%) completed assessments. There were improvements in eating control (11.2 point WEL score change, 95% CI 4.7 to 17.8), step counts (mean change 869 steps/day, 95% CI 198 to 1,540), weight (mean change -2.2%; 95% CI -3.6 to -0.8), and HbA1c (mean change -0.3% HbA1c, 95% CI -0.6 to -0.1), as well as suggestion of systolic blood pressure reduction (mean change -3.5 mm Hg, 95% CI -7.8 to 0.9). Findings were not attributable to medication changes. In linear regression models (adjusted for age, sex, ethnicity, insulin use, season), a -2.5% weight change was associated with a -0.3% HbA1c change (95% CI -0.4 to -0.2) and a -3.5% systolic blood pressure change (95% CI -5.5 to -1.4). In this 'proof of concept' study, persistence with the program led to improvements in eating and physical activity habits, glycemia reductions, and suggestion of blood pressure lowering effects. The strategy thus merits further study and development to expand the range of options for vascular risk reduction in DM2.

  14. Preparation of basil seed mucilage aerogels loaded with paclitaxel nanoparticles by the combination of phase inversion technique and gas antisolvent process

    Directory of Open Access Journals (Sweden)

    Seyyed Ghoreishi

    2017-09-01

    Full Text Available Objective(S: In this work, paclitaxel (PX, a promising anticancer drug, was loaded in the basil seed mucilage (BSM aerogels by implementation of supercritical carbon dioxide (SC-CO2 technology. Then, the effects of operating conditions were studied on the PX mean particle size (MPS, particle size distribution (PSD and drug loading efficiency (DLE. Methods: The employed SC-CO2 process in this research is the combination of phase inversion technique and gas antisolvent (GAS process. The effect of DMSO/water ratio (4 and 6 (v/v, pressure (10-20 MPa, CO2 addition rate (1–3 mL/min and ethanol concentration (5-10% were studied on MPS, PSD and DLE. Scanning electron microscopy (SEM and Zetasizer were used for particle analysis. DLE was investigated by utilizing the high-performance liquid chromatography (HPLC. Results: Nanoparticles of paclitaxel (MPS of 82–131 nm depending on process variables with narrow PSD were successfully loaded in BSM aerogel with DLE of 28–52%. Experimental results indicated that higher DMSO/water ratio, ethanol concentration, pressure and CO2 addition rate reduced MPS and DLE. Conclusions: A modified semi batch SC-CO2 process based on the combination of gas antisolvent process and phase inversion methods using DMSO as co-solvent and ethanol as a secondary solvent was developed for the loading of an anticancer drug, PX, in ocimum basilicum mucilage aerogel. The experimental results determined that the mean particle size, particle size distribution, and drug loading efficiency be controlled with operating conditions.

  15. Phase Vocoder

    Directory of Open Access Journals (Sweden)

    J.L. Flanagan

    2013-08-01

    Full Text Available A vocoder technique is described in which speech signals are represented by their short-time phase and amplitude spectra. A complete transmission system utilizing this approach is simulated on a digital computer. The encoding method leads to an economy in transmission bandwidth and to a means for time compression and expansion of speech signals.

  16. Preparation of fine powdered composite for latent heat storage

    Energy Technology Data Exchange (ETDEWEB)

    Fořt, Jan, E-mail: jan.fort.1@fsv.cvut.cz; Trník, Anton, E-mail: anton.trnik@fsv.cvut.cz; Pavlíková, Milena, E-mail: milena.pavlikova@fsv.cvut.cz; Pavlík, Zbyšek, E-mail: pavlikz@fsv.cvut.cz [Department of Materials Engineering and Chemistry, Faculty of Civil Engineering, Czech Technical University in Prague, Thákurova 7, 166 29 Prague (Czech Republic); Pomaleski, Marina, E-mail: marina-pomaleski@fsv.cvut.cz [Faculty of Civil Engineering, Architecture and Urbanism, University of Campinas, R. Saturnino de Brito 224, 13083-889 Campinas – SP (Brazil)

    2016-07-07

    Application of latent heat storage building envelope systems using phase-change materials represents an attractive method of storing thermal energy and has the advantages of high-energy storage density and the isothermal nature of the storage process. This study deals with a preparation of a new type of powdered phase change composite material for thermal energy storage. The idea of a composite is based upon the impregnation of a natural silicate material by a reasonably priced commercially produced pure phase change material and forming the homogenous composite powdered structure. For the preparation of the composite, vacuum impregnation method is used. The particle size distribution accessed by the laser diffraction apparatus proves that incorporation of the organic phase change material into the structure of inorganic siliceous pozzolana does not lead to the clustering of the particles. The compatibility of the prepared composite is characterized by the Fourier transformation infrared analysis (FTIR). Performed DSC analysis shows potential of the developed composite for thermal energy storage that can be easily incorporated into the cement-based matrix of building materials. Based on the obtained results, application of the developed phase change composite can be considered with a great promise.

  17. Oxygen reduction using platinum electrocatalysts prepared by liquid phase photo-deposition; Reduccion de oxigeno mediante electrocatalizadores de platino preparados por foto-deposicion en fase liquida

    Energy Technology Data Exchange (ETDEWEB)

    Ruiz-Camacho, B.; Perez-Galindo, J. A.; Valenzuela, M. A.; Gonzalez-Huerta, R. G. [Instituto Politecnico Nacional, ESIQIE, Mexico D.F. (Mexico)]. E-mail: rosgonzalez_h@yahoo.com.mx

    2009-09-15

    This work presents the synthesis and characterization of nanometric-sized Pt/C electrochemical catalysts using impregnation and liquid phase photo-deposition methods. Two platinum precursors were used, C{sub 10}H{sub 14}O{sub 4}Pt (Pt acetylacetonate, Pt(acac){sub 2}) and H{sub 2}PtCl{sub 6} (hexachloroplatinic acid) to study the effect on the particle size and the electrocatalytic behavior in the oxygen reduction reaction. The characterization of the catalysts was done using x-ray diffraction, hydrogen chemisorption and transmission electron microscopy. The electrochemical study was conducted with cyclic voltamperometry and rotary disc electrode (RDE) techniques. Pt (E-tek) was used as a reference catalyst. The peaks of the platinum were identified based on the x-ray diffraction results, and correspond to crystalline phases (111) and (200), whose intensity was greater when using H{sub 2}PtCl{sub 6} versus Pt(acac){sub 2}. The hydrogen chemisorption and transmission electron microscopy tests found that the larger-sized particle (1-5 nm) and greater metallic dispersion was obtained using Pt(acac){sub 2} as a platinum precursor and liquid phase photo-deposition. It was also found that this material presented the best electrochemical response, showing a open-circuit potential of 0.96 V and over-potential of 0.05 V with respect to H{sub 2}PtCl{sub 6} and of 0.22 V with respect to the catalyst obtained using impregnation. [Spanish] En este trabajo se presenta la sintesis y caracterizacion electroquimica de catalizadores de tamano nanometrico de Pt/C empleando los metodos de impregnacion y foto-deposicion en fase liquida. Se utilizaron dos precursores del platino C{sub 10}H{sub 14}O{sub 4}Pt (acetil-acetonato de Pt, Pt(acac){sub 2}) y H2PtCl6 (acido hexacloroplatinico), para estudiar el efecto que tienen sobre el tamano de particula y el comportamiento electrocatalitico en la reaccion de reduccion de oxigeno. La caracterizacion de los catalizadores se realizo mediante

  18. Preparation, thermal and flammability properties of a novel form-stable phase change materials based on high density polyethylene/poly(ethylene-co-vinyl acetate)/organophilic montmorillonite nanocomposites/paraffin compounds

    International Nuclear Information System (INIS)

    Cai Yibing; Song Lei; He Qingliang; Yang Dandan; Hu Yuan

    2008-01-01

    The paraffin is one of important thermal energy storage materials with many desirable characteristics (i.e., high heat of fusion, varied phase change temperature, negligible supercooling, self-nucleating, no phase segregation and cheap, etc.), but has low thermal stability and flammable. Hence, a novel form-stable phase change materials (PCM) based on high density polyethylene (HDPE)/poly(ethylene-co-vinyl acetate) (EVA)/organophilic montmorillonite (OMT) nanocomposites and paraffin are prepared by twin-screw extruder technique. The structures of the HDPE-EVA/OMT nanocomposites and the form-stable PCM are evidenced by the X-ray diffraction (XRD), transmission electronic microscopy (TEM) and scanning electronic microscope (SEM). The results of XRD and TEM show that the HDPE-EVA/OMT nanocomposites form the ordered intercalated nanomorphology. The form-stable PCM consists of the paraffin, which acts as a dispersed phase change material and the HDPE-EVA/OMT nanocomposites, which acts as the supporting material. The paraffin disperses in the three-dimensional net structure formed by HDPE-EVA/OMT nanocomposites. The thermal stability, latent heat and flammability properties are characterized by thermogravimetry analysis (TGA), dynamic Fourier-transform infrared (FTIR), differential scanning calorimeter (DSC) and cone calorimeter, respectively. The TGA and dynamic FTIR analyses indicate that the incorporation of suitable amount of OMT into the form-stable PCM increase the thermal stability. The DSC results show that the latent heat of the form-stable PCM has a certain degree decrease. The cone calorimeter shows that the heat release rate (HRR) has remarkably decreases with loading of OMT in the form-stable PCM, contributing to the improved flammability properties

  19. Adsorptive removal of organics from aqueous phase by acid-activated coal fly ash: preparation, adsorption, and Fenton regenerative valorization of "spent" adsorbent.

    Science.gov (United States)

    Wang, Nannan; Hao, Linlin; Chen, Jiaqing; Zhao, Qiang; Xu, Han

    2018-05-01

    Raw coal fly ash was activated to an adsorbent by sulfuric acid impregnation. The activation condition, the adsorption capacity, and the regenerative valorization of the adsorbent were studied. The results show that the optimal preparation conditions of the adsorbent are [H 2 SO 4 ] = 1 mol L -1 , activation time = 30 min, the ratio of coal fly ash to acid = 1:20 (g:mL), calcination temperature = 100 °C. The adsorption of p-nitrophenol on the adsorbent accords with the pseudo-second-order kinetic equation and the adsorption rate constant is 0.089 g mg -1  min -1 . The adsorption on this adsorbent can be considered enough after 35 min, when the corresponding adsorption capacity is 1.07 mg g -1 (85.6% of p-nitrophenol removal). Compared with raw coal fly ash, the adsorbent has a stable adsorption performance at low pH range (pH = 1-6) and the adsorption of p-nitrophenol is an exothermic process. Ninety minutes is required for the regenerative valorization of saturated adsorbent by Fenton process. The regenerative valorization for this saturated adsorbent can reach 89% under the optimal proposed conditions (30 °C, pH = 3, [H 2 O 2 ] = 5.0 mmol L -1 , [Fe 2+ ] = 5.5 mmol L -1 ). Within 15 experimental runs, the adsorbent has a better and better stability with the increase of experimental runs. Finally, the mechanism of activating coal fly ash is proposed, being verified by the results of the SEM and BET test.

  20. Preparation and characterization of magnetic allylamine modified graphene oxide-poly(vinyl acetate-co-divinylbenzene) nanocomposite for vortex assisted magnetic solid phase extraction of some metal ions.

    Science.gov (United States)

    Khan, Mansoor; Yilmaz, Erkan; Sevinc, Basak; Sahmetlioglu, Ertugrul; Shah, Jasmin; Jan, Muhammad Rasul; Soylak, Mustafa

    2016-01-01

    Magnetic allylamine modified graphene oxide-poly(vinyl acetate-co-divinylbenzene) (MGO-DVB-VA) was synthesized and used for magnetic solid phase extraction of Pb(II), Cd(II), Cu(II), Ni(II) and Co(II) prior to their determination by flame atomic absorption spectroscopy. The adsorbent surface functional group was characterized by using FT-IR and Raman spectroscopy. XRD pattern was used to determine the layers of GO. Surface morphology and elemental composition of the adsorbent were evaluated by using SEM and EDX analysis. Various parameters, effecting adsorption efficiency like initial solution pH, adsorbent dose, type and volume of eluent, volume of sample and diverse ions effects were optimized. The preconcentration factor (PF) is 40 for all the metals and the limits of detection for Pb, Cd, Cu, Ni and Co are in the range of 0.37-2.39 µg L(-1) and relative standard deviation below 3.1%. The method was validated by using the method for certified reference materials (Tobacco Leaves (INCT-OBTL-5), Tomato Leaves (1573a), Certified Water (SPS-ww2) and Certified Water (TMDA 64-2)). The method was successfully applied for natural water and food samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Sonochemical synthesis and characterization of nano-sized zinc(II coordination complex as a precursor for the preparation of pure-phase zinc(II oxide nanoparticles

    Directory of Open Access Journals (Sweden)

    Maryam Ranjbar

    2017-01-01

    Full Text Available In current study, nanoparticles and single crystals of a Zn(II coordination complex, [Zn(dmphI2](1, {dmph=2,9-dimethyl-1,10-phenanthroline(neocuproine}, have been synthesized by the reaction of zinc(II acetate, KI and neocuproine as ligand in methanol using sonochemical and heat gradient methods, respectively. The nanostructure of 1 was characterized by scanning electron microscopy (SEM, X-ray powder diffraction (XRD, FT-IR spectroscopy and elemental analyses, and the structure of compound 1 was determined by single-crystal X-ray diffraction. The thermal stability of nano-sized 1 has been studied by thermogravimetric (TG and differential thermal analyses (DTA. Structural determination of compound 1 reveals the Zn(II ion is four-coordinated in a distorted tetrahedral configuration by two N atoms from a 2,9-dimethyl-1,10-Phenanthroline ligand and two terminal I atoms. The effect of supercritical condition on stability, size and morphology of nano-structured compound 1 has also been studied. The XRD pattern of the residue obtained from thermal decomposition of nano-sized compound 1 at 600 °C under air atmosphere provided pure phase of ZnO with the average particles size of about 31 nm.

  2. Preparation of an aminopropyl imidazole-modified silica gel as a sorbent for solid-phase extraction of carboxylic acid compounds and polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Wang, Na; Guo, Yong; Wang, Licheng; Liang, Xiaojing; Liu, Shujuan; Jiang, Shengxiang

    2014-05-21

    In this paper, a kind of aminopropyl imidazole-modified silica sorbent was synthesized and used as a solid-phase extraction (SPE) sorbent for the determination of carboxylic acid compounds and polycyclic aromatic hydrocarbons (PAHs). The resultant aminopropyl imidazole-modified silica sorbent was characterized by Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to ensure the successful binding of aminopropyl imidazole on the surface of silica gel. Then the aminopropyl imidazole-modified silica sorbent served as a SPE sorbent for the enrichment of carboxylic acid compounds and PAHs. The new sorbent exhibited high extraction efficiency towards the tested compounds and the results show that such a sorbent can offer multiple intermolecular interactions: electrostatic, π-π, and hydrophobic interactions. Several parameters affecting the extraction recovery, such as the pH of sample solution, the pH of eluent, the solubility of eluent, the volume of eluent, and sample loading, were also investigated. Under the optimized conditions, the proposed method was applied to the analysis of four carboxylic acid compounds and four PAHs in environmental water samples. Good linearities were obtained for all the tested compounds with R(2) larger than 0.9903. The limits of detection were found to be in the range of 0.0065-0.5 μg L(-1). The recovery values of spiked river water samples were from 63.2% to 112.3% with relative standard deviations (RSDs) less than 10.1% (n = 4).

  3. In situ fabrication of nanostructured titania coating on the surface of titanium wire: A new approach for preparation of solid-phase microextraction fiber

    International Nuclear Information System (INIS)

    Cao Dandan; Lue Jianxia; Liu Jingfu; Jiang Guibin

    2008-01-01

    Nanostructured titania-based solid-phase microextraction (SPME) fibers were fabricated through the in situ oxidation of titanium wires with H 2 O 2 (30%, w/w) at 80 deg. C for 24 h. The obtained SPME fibers possess a ∼1.2 μm thick nanostructured coating consisting of ∼100 nm titania walls and 100-200 nm pores. The use of these fibers for headspace SPME coupled with gas chromatography with electron capture detection (GC-ECD) resulted in improved analysis of dichlorodiphenyltrichloroethane (DDT) and its degradation products. The presented method to detect DDT and its degradation products has high sensitivity (0.20-0.98 ng L -1 ), high precision (relative standard deviation R.S.D. = 9.4-16%, n = 5), a wide linear range (5-5000 ng L -1 ), and good linearity (coefficient of estimation R 2 = 0.991-0.998). As the nanostructured titania was in situ formed on the surface of a titanium wire, the coating was uniformly and strongly adhered on the titanium wire. Because of the inherent chemical stability of the titania coating and the mechanical durability of the titanium wire substrate, this new SPME fiber exhibited long life span (over 150 times)

  4. In situ fabrication of nanostructured titania coating on the surface of titanium wire: A new approach for preparation of solid-phase microextraction fiber

    Energy Technology Data Exchange (ETDEWEB)

    Cao Dandan [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China); Environmental Science Division, School of Earth and Space Science, University of Science and Technology of China, Hefei, Anhui Province 230026 (China); Lue Jianxia [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China); Liu Jingfu [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China)], E-mail: jfliu@rcees.ac.cn; Jiang Guibin [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China)

    2008-03-17

    Nanostructured titania-based solid-phase microextraction (SPME) fibers were fabricated through the in situ oxidation of titanium wires with H{sub 2}O{sub 2} (30%, w/w) at 80 deg. C for 24 h. The obtained SPME fibers possess a {approx}1.2 {mu}m thick nanostructured coating consisting of {approx}100 nm titania walls and 100-200 nm pores. The use of these fibers for headspace SPME coupled with gas chromatography with electron capture detection (GC-ECD) resulted in improved analysis of dichlorodiphenyltrichloroethane (DDT) and its degradation products. The presented method to detect DDT and its degradation products has high sensitivity (0.20-0.98 ng L{sup -1}), high precision (relative standard deviation R.S.D. = 9.4-16%, n = 5), a wide linear range (5-5000 ng L{sup -1}), and good linearity (coefficient of estimation R{sup 2} = 0.991-0.998). As the nanostructured titania was in situ formed on the surface of a titanium wire, the coating was uniformly and strongly adhered on the titanium wire. Because of the inherent chemical stability of the titania coating and the mechanical durability of the titanium wire substrate, this new SPME fiber exhibited long life span (over 150 times)

  5. Water-compatible dummy molecularly imprinted resin prepared in aqueous solution for green miniaturized solid-phase extraction of plant growth regulators.

    Science.gov (United States)

    Wang, Mingyu; Chang, Xiaochen; Wu, Xingyu; Yan, Hongyuan; Qiao, Fengxia

    2016-08-05

    A water-compatible dummy molecularly imprinted resin (MIR) was synthesized in water using melamine, urea, and formaldehyde as hydrophilic monomers of co-polycondensation. A triblock copolymer (PEO-PPO-PEO, P123) was used as porogen to dredge the network structure of MIR, and N-(1-naphthyl) ethylenediamine dihydrochloride, which has similar shape and size to the target analytes, was the dummy template of molecular imprinting. The obtained MIR was used as the adsorbent in a green miniaturized solid-phase extraction (MIR⬜mini-SPE) of plant growth regulators, and there was no organic solvent used in the entire MIR⬜mini-SPE procedure. The calibration linearity of MIR⬜mini-SPE⬜HPLC method was obtained in a range 5⬜250ngmL(↙1) for IAA, IPA, IBA, and NAA with correlation coefficient (r) Ⱕ0.9998. Recoveries at three spike levels are in the range of 87.6⬜100.0% for coconut juice with relative standard deviations Ⱔ8.1%. The MIR⬜mini-SPE method possesses the advantages of environmental friendliness, simple operation, and high efficiency, so it is potential to apply the green pretreatment strategy to extraction of trace analytes in aqueous samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. 1D TiO2 Nanostructures Prepared from Seeds Presenting Tailored TiO2 Crystalline Phases and Their Photocatalytic Activity for Escherichia coli in Water

    Directory of Open Access Journals (Sweden)

    Julieta Cabrera

    2018-01-01

    Full Text Available TiO2 nanotubes were synthesized by alkaline hydrothermal treatment of TiO2 nanoparticles with a controlled proportion of anatase and rutile. Tailoring of TiO2 phases was achieved by adjusting the pH and type of acid used in the hydrolysis of titanium isopropoxide (first step in the sol-gel synthesis. The anatase proportion in the precursor nanoparticles was in the 3–100% range. Tube-like nanostructures were obtained with an anatase percentage of 18 or higher while flake-like shapes were obtained when rutile was dominant in the seed. After annealing at 400°C for 2 h, a fraction of nanotubes was conserved in all the samples but, depending on the anatase/rutile ratio in the starting material, spherical and rod-shaped structures were also observed. The photocatalytic activity of 1D nanostructures was evaluated by measuring the deactivation of E. coli in stirred water in the dark and under UV-A/B irradiation. Results show that in addition to the bactericidal activity of TiO2 under UV-A illumination, under dark conditions, the decrease in bacteria viability is ascribed to mechanical stress due to stirring.

  7. Preparation and characterization of sodium dodecyl sulfate doped polypyrrole solid phase micro extraction fiber and its application to endocrine disruptor pesticide analysis.

    Science.gov (United States)

    Korba, Korcan; Pelit, Levent; Pelit, Füsun Okçu; Ozdokur, K Volkan; Ertaş, Hasan; Eroğlu, Ahmet E; Ertaş, F Nil

    2013-06-15

    A robust in house solid-phase micro extraction (SPME) surface has been developed for the headspace (HS)-SPME determination of endocrine disruptor pesticides, namely, Chlorpyrifos, Penconazole, Procymidone, Bromopropylate and Lambda-Cyhalothrin in wine sample by using sodium dodecylsulfate doped polypyrrole SPME fiber. Pyrrole monomer was electrochemically polymerized on a stainless steel wire in laboratory conditions in virtue of diminishing the cost and enhancing the analyte retention on its surface to exert better selectivity and hence the developed polymerized surface could offer to analyst to exploit it as a fiber in headspace SPME analysis. The parameters, mainly, adsorption temperature and time, desorption temperature, stirring rate and salt amount were optimized to be as 70°C and 45min, 200°C, 600rpm and 10gL(-1), respectively. Limit of detection was estimated in the range of 0.073-1.659ngmL(-1) for the pesticides studied. The developed method was applied in to red wine sample with acceptable recovery values (92-107%) which were obtained for these selected pesticides. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. 蓄热调温纤维用DA@PMMA相变微胶囊的制备及表征%Preparation and characterization of n-dodecyl alcohol/polymethyl methacrylate phase change microencapsules used in thermo-regulating fibre

    Institute of Scientific and Technical Information of China (English)

    黄明; 罗艳; 钟毅; 肖敏; 胡剑灿

    2017-01-01

    Due to the phase change temperature (about 22 ℃) of n- dodecyl alcohol (DA) was in the com?fortable temperature range (18~28 ℃) of human body, it was selected as the core material, and polymethyl?methacrylate (PMMA) as wall material, DA@PMMA phase change microcapsules was prepared by in- situ po?lymerization method. The morphologies, particle size distribution, chemical composition, thermal and compres?sive properties of resulted microcapsules was characterized by scanning electron microscopy (SEM), laser parti?cle size analyzer, differential scanning calorimetry (DSC), thermogravimetric analysis (TG) and compression ma?chine, respectively. It was found that the mean particle size of microcapsules was about 1.232 μm. The sur?face of DA@PMMA microcapsules was smooth and compact. The range of phase change temperature of DA@PMMA microcapsules was 18.7~25 ℃. In addition, their phase change enthalpy was up to 92.3 J/g and the encapsulation efficiency was 84.7%. DA@PMMA microcapsules had good resistance to pressure, which was suitable to prepare thermo- regulating fibre.%基于正十二醇(DA)相变温度(约22℃)处于人体最佳舒适温度18~28℃范围内,采用DA为相变芯材,聚甲基丙烯酸甲酯(PMMA)为包封壁材,通过原位聚合法制备蓄热调温纺织品纤维用DA@PMMA相变微胶囊,并对相变微胶囊的形貌、粒径分布、热性能及抗压性进行表征.结果表明:DA@PMMA相变微胶囊粒径分布集中于1.232μm附近;壁材表面光滑致密;相变温度为18.7~25℃,热焓值为92.3 J/g,芯材包封率为84.7%,且具有较好的抗压性;可用于制备蓄热调温纺织品纤维.

  9. Preparation, characterization, and applications of a novel solid-phase microextraction fiber by sol-gel technology on the surface of stainless steel wire for determination of poly cyclic aromatic hydrocarbons in aquatic environmental samples

    International Nuclear Information System (INIS)

    Es-haghi, Ali; Hosseininasab, Valiallah; Bagheri, Habib

    2014-01-01

    Graphical abstract: - Highlights: • A novel solid-phase microextraction (SPME) fiber was prepared using sol–gel technology. • Sol–gel coating was performed on stainless steel substrate. • The new fibers are robust and unbreakable with temperature stability. • The fibers were used for extraction of PAHs from aqueous samples. - Abstract: A novel solid-phase microextraction(SPME) fiber was prepared using sol–gel technology with ethoxylated nonylphenol as a fiber coating material. The fiber was employed to develop a headspace SPME–GC–MS method suitable for quantification of 13 polycyclic aromatic hydrocarbons (PAHs) in water samples. Surface characteristics of the fibers were inspected by energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The SEM measurements showed the presence of highly porous nano-sized particles in the coating. Important parameters affecting the extraction efficiency such as extraction temperature and time, desorption conditions as well as ionic strength have been evaluated and optimized. In the next step, the validation of the new method have been performed, finding it to be specific in the trace analysis of PAHs, with the limit of detection (LOD) ranging from 0.01 to 0.5 μg L −1 and the linear range from the respective LOD to 200 μg L −1 with RSD amounting to less than 8%. The thermal stability of the fibers was investigated as well and they were found to be durable at 280 °C for 345 min. Furthermore, the proposed method was successfully applied for quantification of PAHs in real water samples

  10. Preparation, characterization, and applications of a novel solid-phase microextraction fiber by sol-gel technology on the surface of stainless steel wire for determination of poly cyclic aromatic hydrocarbons in aquatic environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Es-haghi, Ali, E-mail: a.eshaghi@rvsri.ac.ir [Department of Physico Chemistry, Razi Vaccine and Serum Research Institute, PO Box 31975/148, Karaj (Iran, Islamic Republic of); Hosseininasab, Valiallah; Bagheri, Habib [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, PO Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2014-02-01

    Highlights: • A novel solid-phase microextraction (SPME) fiber was prepared using sol–gel technology. • Sol–gel coating was performed on stainless steel substrate. • The new fibers are robust and unbreakable with temperature stability. • The fibers were used for extraction of PAHs from aqueous samples. Abstract: A novel solid-phase microextraction(SPME) fiber was prepared using sol–gel technology with ethoxylated nonylphenol as a fiber coating material. The fiber was employed to develop a headspace SPME–GC–MS method suitable for quantification of 13 polycyclic aromatic hydrocarbons (PAHs) in water samples. Surface characteristics of the fibers were inspected by energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The SEM measurements showed the presence of highly porous nano-sized particles in the coating. Important parameters affecting the extraction efficiency such as extraction temperature and time, desorption conditions as well as ionic strength have been evaluated and optimized. In the next step, the validation of the new method have been performed, finding it to be specific in the trace analysis of PAHs, with the limit of detection (LOD) ranging from 0.01 to 0.5 μg L⁻¹ and the linear range from the respective LOD to 200 μg L⁻¹with RSD amounting to less than 8%. The thermal stability of the fibers was investigated as well and they were found to be durable at 280 °C for 345 min. Furthermore, the proposed method was successfully applied for quantification of PAHs in real water samples.

  11. Preparation of ionic liquid modified magnetic metal-organic frameworks composites for the solid-phase extraction of α-chymotrypsin.

    Science.gov (United States)

    Wei, Xiaoxiao; Wang, Yuzhi; Chen, Jing; Xu, Panli; Zhou, Yigang

    2018-05-15

    A novel magnetic solid-phase extraction (MSPE) method based on 1-hexyl-3-methyl imidazolium chloride ionic liquid (IL) modified magnetic Fe 3 O 4 nanoparticles, hydroxylated multiwall carbon nanotubes (MWCNTs-OH) and zeolitic imidazolate frameworks (ZIFs) nanocomposites (Fe 3 O 4 -MWCNTs-OH@ZIF-67@IL) were proposed and applied to extract α-chymotrypsin. The magnetic materials were synthesized successfully and characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), thermal gravimetric analysis (TGA), fourier transform infrared spectrometry (FT-IR), vibrating sample magnetometer (VSM) and zeta potentials. Subsequently, the UV-vis spectrophotometer at about 280 nm was utilized to quantitatively analyze the α-chymotrypsin concentration in the supernatant. Furthermore, single factor experiments revealed that the extraction capacity was influenced by initial α-chymotrypsin concentration, ionic strength, extraction time, extraction temperature and pH value. The extraction capacity could reach up to about 635 mg g -1 under the optimized conditions, absolutely higher than that of extraction for Ovalbumin (OVA), Bovine serum albumin (BSA) and Bovine hemoglobin (BHb). In addition, the regeneration studies showed Fe 3 O 4 -MWCNTs-OH@ZIF-67@IL particles could be reused several times and kept a high extraction capacity. Besides, the study of enzymatic activity also indicated that the activity of the extracted α-chymotrypsin was well maintained 93% of initial activity. What's more, the proposed method was successfully applied to extract α-chymotrypsin in porcine pancreas crude extract with satisfactory results. All of above conclusions highlight the great potential of the proposed Fe 3 O 4 -MWCNTs-OH@ZIF-67@IL-MSPE method in the analysis of biomolecules. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Effect of sonochemical synthesized TiO2 nanoparticles and coagulation bath temperature on morphology, thermal stability and pure water flux of asymmetric cellulose acetate membranes prepared via phase inversion method

    Directory of Open Access Journals (Sweden)

    Abedini Reza

    2012-01-01

    Full Text Available In this study, asymmetric pure CA and CA/ TiO2 composite membranes were prepared via phase inversion by dispersing TiO2 nanopaticles in the CA casting solutions induced by immersion precipitation in water coagulation bath. TiO2 nanoparticles, which were synthesized by the sonochemical method, were added into the casting solution with different concentrations. Effects of TiO2 nanoparticles concentration (0 wt. %, 5wt.%, 10wt.%, 15wt.%, 20wt.% and 25wt.% and coagulation bath temperature (CBT= 25°C, 50°C and 75°C on morphology, thermal stability and pure water flux (PWF of the prepared membranes were studied and discussed. Increasing TiO2 concentration in the casting solution film along with higher CBT resulted in increasing the membrane thickness, water content (WC, membrane porosity and pure water flux (PWF, also these changes facilitate macrovoids formation. Thermal gravimetric analysis (TGA shows that thermal stability of the composite membranes were improved by the addition of TiO2 nanopaticles. Also TGA results indicated that increasing CBT in each TiO2 concentration leads to the decreasing of decomposition temperature (Td of hybrid membranes.

  13. Personnel Preparation.

    Science.gov (United States)

    Fair, George, Ed.; Stodden, Robert, Ed.

    1981-01-01

    Three articles comprise a section on personnel preparation in vocational education. Articles deal with two inservice programs in career/vocational education for the handicapped and a project to train paraprofessionals to assist special educators in vocational education. (CL)

  14. Yucca Mountain Climate Technical Support Representative

    International Nuclear Information System (INIS)

    Sharpe, Saxon E

    2007-01-01

    The primary objective of Project Activity ORD-FY04-012, 'Yucca Mountain Climate Technical Support Representative', was to provide the Office of Civilian Radioactive Waste Management (OCRWM) with expertise on past, present, and future climate scenarios and to support the technical elements of the Yucca Mountain Project (YMP) climate program. The Climate Technical Support Representative was to explain, defend, and interpret the YMP climate program to the various audiences during Site Recommendation and License Application. This technical support representative was to support DOE management in the preparation and review of documents, and to participate in comment response for the Final Environmental Impact Statement, the Site Recommendation Hearings, the NRC Sufficiency Comments, and other forums as designated by DOE management. Because the activity was terminated 12 months early and experience a 27% reduction in budget, it was not possible to complete all components of the tasks as originally envisioned. Activities not completed include the qualification of climate datasets and the production of a qualified technical report. The following final report is an unqualified summary of the activities that were completed given the reduced time and funding

  15. Diversity and representativeness: two key factors

    CERN Multimedia

    Staff Association

    2013-01-01

    In the past few weeks many of you have filled out the questionnaire for preparing the upcoming Five-yearly review. Similarly, Staff Association members have elected their delegates to the Staff Council for the coming two years. Once again we would like to thank all those who have taken the time and effort to make their voice heard on these two occasions. Elections to the Staff Council Below we publish the new Staff Council with its forty delegates who will represent in 2014 and 2015 all CERN staff in the discussions with Management and Member States in the various bodies and committees. Therefore it is important that the Staff Council represents as far as possible the diversity of the CERN population. By construction, the election process with its electoral colleges and two-step voting procedure guarantees that all Departments, even the small ones, and the various staff categories are correctly represented. Figure 1 shows the participation rate in the elections. The average rate is just above 52 %, with ...

  16. Representative process sampling - in practice

    DEFF Research Database (Denmark)

    Esbensen, Kim; Friis-Pedersen, Hans Henrik; Julius, Lars Petersen

    2007-01-01

    Didactic data sets representing a range of real-world processes are used to illustrate "how to do" representative process sampling and process characterisation. The selected process data lead to diverse variogram expressions with different systematics (no range vs. important ranges; trends and....../or periodicity; different nugget effects and process variations ranging from less than one lag to full variogram lag). Variogram data analysis leads to a fundamental decomposition into 0-D sampling vs. 1-D process variances, based on the three principal variogram parameters: range, sill and nugget effect...

  17. Direct preparation of a graphene oxide modified monolith in a glass syringe as a solid-phase extraction cartridge for the extraction of quaternary ammonium alkaloids from Chinese patent medicine.

    Science.gov (United States)

    Liang, Xiaojing; Wang, Licheng; Wang, Shuai; Li, Yijing; Guo, Yong

    2017-11-01

    Packed cartridges have been widely used in solid-phase extraction. However, there are still some drawbacks, such as they are blocked easily and the method is time-consuming. In view of the advantages of monoliths, a monolithic extraction material has been directly synthesized in a glass syringe without any gap between the monolith and syringe inner wall. The monolithic syringe was modified with graphene oxide by loading graphene oxide dispersion onto it. The content of graphene oxide and the surface topography of the monolith have been evaluated by elemental analysis and scanning electron microscopy, respectively, which confirmed the successful modification. This prepared graphene oxide-modified monolithic syringe was directly used as a traditional solid-phase extraction cartridge. As expected, it shows good permeability and excellent capability for the extraction of quaternary ammonium alkaloids. The sample loading velocity (1-6 mL/min) does not affect the recovery. Under the optimal conditions, good linearities (R = 0.9992-0.9998) were obtained for five quaternary ammonium alkaloids, and the limits of detection and quantification were 0.5-1 and 1-2 μg/L, respectively. The proposed method was successfully applied for the analysis of quaternary ammonium alkaloids in Chinese patent medicine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Effect of electron irradiation exposure on phase formation, microstructure and mechanical strength of Bi{sub 2}Sr{sub 2}CaCu{sub 2}O{sub 8} superconductor prepared via co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Mohiju, Zaahidah ' Atiqah; Hamid, Nasri A., E-mail: Nasri@uniten.edu.my; Kannan, V. [Center for Nuclear Energy, College of Engineering, Universiti Tenaga Nasional, Jalan IKRAM-UNITEN, 43000 Kajang, Selangor (Malaysia); Abdullah, Yusof [Materials Technology Group, Industrial Technology Division, Malaysian Nuclear Agency, Bangi, 43000 Kajang, Selangor (Malaysia)

    2015-04-29

    In this work the effect of electron irradiation on the mechanical properties of Bi2Sr2CaCu2O8 (Bi-2212) superconductor was studied by exposing the Bi-2212 superconductor with different doses of electron irradiation. Bi-2212 samples were prepared by using co-precipitation method. Irradiation was performed with irradiation dose of 100 kGray and 200 kGray, respectively. Characterization of the samples was performed by using X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). Instron Universal Testing machine was used to measure the strength of the samples. The XRD patterns for the non-irradiated and irradiated samples show well-defined peaks of which could be indexed on the basis of a Bi-2212 phase structure. XRD patterns also indicate that electron irradiation did not affect the Bi-2212 superconducting phase. SEM micrographs show disorientation in the texture of the microstructure for irradiated samples. Sample exposed to 200 kGray electron irradiation dose shows enhancement of grain size. Their grain growth and texture improved slightly compared to other sample. The results also show that enlargement of grain size resulted in higher mechanical strength.

  19. Solution preparation

    International Nuclear Information System (INIS)

    Seitz, M.G.

    1982-01-01

    Reviewed in this statement are methods of preparing solutions to be used in laboratory experiments to examine technical issues related to the safe disposal of nuclear waste from power generation. Each approach currently used to prepare solutions has advantages and any one approach may be preferred over the others in particular situations, depending upon the goals of the experimental program. These advantages are highlighted herein for three approaches to solution preparation that are currently used most in studies of nuclear waste disposal. Discussion of the disadvantages of each approach is presented to help a user select a preparation method for his particular studies. Also presented in this statement are general observations regarding solution preparation. These observations are used as examples of the types of concerns that need to be addressed regarding solution preparation. As shown by these examples, prior to experimentation or chemical analyses, laboratory techniques based on scientific knowledge of solutions can be applied to solutions, often resulting in great improvement in the usefulness of results

  20. Marc Treib: Representing Landscape Architecture

    DEFF Research Database (Denmark)

    Braae, Ellen Marie

    2008-01-01

    The editor of Representing Landscape Architecture, Marc Treib, argues that there is good reason to evaluate the standard practices of representation that landscape architects have been using for so long. In the rush to the promised land of computer design these practices are now in danger of being...

  1. Does representative wind information exist?

    NARCIS (Netherlands)

    Wieringa, J.

    1996-01-01

    Representativity requirements are discussed for various wind data users. It is shown that most applications can be dealt with by using data from wind stations when these are made to conform with WMO specifications. Methods to achieve this WMO normalization are reviewed, giving minimum specifications

  2. OAS :: Member States : Permanent Representatives

    Science.gov (United States)

    Rights Actions against Corruption C Children Civil Registry Civil Society Contact Us Culture Cyber Barbados Belize Bolivia Brazil Canada Chile Colombia Costa Rica Cuba 1 Dominica (Commonwealth of) Dominican Gutierez Ambassador, Permanent Representative of Belize Diego Pary Rodríguez Bolivia Diego Pary Rodríguez

  3. Judgments of and by Representativeness

    Science.gov (United States)

    1981-05-15

    p. 4i). This hy- pothesis was studied in several contexts, including intuitive statisti- cal judgments and the prediction of professional choice (Kahneman... professional choice . Here, X is representative of M either because it is frequently associated with M (e.g., high fever commonly accompanies pneumonia

  4. WIPP facility representative program plan

    International Nuclear Information System (INIS)

    1994-01-01

    This plan describes the Department of Energy (DOE), Carlsbad Area Office (CAO) facility representative (FR) program at the Waste Isolation Pilot Plant (WIPP). It provides the following information: (1) FR and support organization authorities and responsibilities; (2) FR program requirements; and (3) FR training and qualification requirements

  5. Thermal behavior and phase transformation of ZrO2–10%SiO2 precursor powder prepared by a co-precipitation route without adding stability agent

    International Nuclear Information System (INIS)

    Chu, Hsueh-Liang; Hwang, Weng-Sing; Wang, Cheng-Li; Wang, Moo-Chin; Lee, Kuen-Chan; Huang, Hong-Hsin; Lee, Huey-Er

    2014-01-01

    Highlights: • The precursor powders contained about 68.3 wt% ZrO 2 , which corresponds to ZrO 2 ·1/8 H 2 O. • The exothermic peak temperature of tetragonal ZrO 2 formation occurred at 1014 K. • The activation energy of ZrO 2 –10%SiO 2 precursors crystallization is 993.7 kJ/mol. • Only the tetragonal ZrO 2 formed when the precursor calcined at 1173–1373 K for 2 h. • As calcined at 1473 K for 2 h, tetragonal ZrO 2 fully converted to monoclinic ZrO 2 . - Abstract: Thermal behavior and phase transformation of ZrO 2 –10%SiO 2 precursor powder prepared by a co-precipitation route without adding stability agent has been studied using different thermal analysis/thermogravimetry (DTA/TG), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), nano beam electron diffraction (NBED), high-resolution TEM (HRTEM) and energy-dispersive X-ray spectrometer (EDS). The TG results show that four weight loss regions were from 298 to 443 K, 443 to 743 K, 743 to 793 K and 793 to 1400 K. The DTA result shows that the ZrO 2 freeze-dried precursor powders crystallization at 1014 K. The activation energy of 993.7 kJ/mol was obtained for tetragonal ZrO 2 crystallization using a non-isothermal process. The XRD result shows that only a single phase of tetragonal ZrO 2 appears when the freeze-dried precursor powders after calcination between 1173 and 1373 K for 2 h. Moreover, when calcined at 1473 K for 2 h, the phase transformation from tetragonal ZrO 2 fully converted to monoclinic ZrO 2 occurred

  6. Preparation to exceptional operations

    International Nuclear Information System (INIS)

    Sort, M.

    1984-01-01

    Preparation to special maintenance operations requires a specific approach according to the considered intervention type. Replacement of vapor generators is representative of a kind of intervention where technics is generally only an adaptation to the power plant context of processes already in application in construction, and where methodology, planning and organization have an important role because of the variety and the quantity of taskworks to be done, the involved manpower, the dosimetry and time lag requirements [fr

  7. Burnout in Customer Service Representatives

    Directory of Open Access Journals (Sweden)

    Tariq Jalees

    2008-09-01

    Full Text Available The purpose and aim of this research was to (1 identify the factors that contributes towards job burnout in sales service representative (2 What are the relationships of these factors (3 To empirically test the relationships of the determinants relating to burnout in customer service representatives. Based on literature survey six different variables related to burnout were identified. The variables were (1 Emotional exhaustion.(2 Reduced personal accomplishment.(3 Job induced tension.(4 Job satisfaction.(5 Workload (6 Job satisfaction.Each of the variables contained 3 sub-variables. Five different hypotheses were developed and tested through techniques such as Z-test, F-test and regression analysis. The questionnaire administered for the study contained 15 questions including personal data. The subject was Moblink company customers sales service representative in Karachi.The valid sample size was 98 drawn through multi-cluster technique. Techniques such as measure of dispersion and measure of central tendencies were used for analyzing the data. Regression, Z-test, and F-test were used for testing the developed hypothesis.According to the respondents’ opinions, the reduced personal accomplishment had a high rating with a mean of 3.75 and job induced tension has the lowest mean of 3.58. The standard deviation of respondents’ opinions was highest for dimension depersonalization and least for dimension work load. This indicates that there is a high polarization of the respondents’ opinions on the dimension depersonalization moral and least on the dimension work load.The Skew nesses for all the dimensions were in negative except the determinants emotional exhaustion and workload. This indicates that the majority of respondents’ opinions on all the dimensions were below the mean except in the case of emotional exhaustion and workload.Five hypotheses were developed and tested:a The hypothesis relating to low level of burnout in customers

  8. Preparation and Characterization of Glycerol Modified Polyurea Microencapsulated Phase Change Material%丙三醇改性聚脲微胶囊相变材料的研制与性能

    Institute of Scientific and Technical Information of China (English)

    唐易达; 马志鹏; 陆少锋

    2012-01-01

    以硬脂酸丁酯为芯材,苯乙烯马来酸酐共聚物(SMA)为乳化分散剂,以单体2,4-甲苯二异氰酸酯(TDI)和二亚乙基三胺(EDTA)反应并采用丙三醇进行改性形成的聚脲树脂为壳体,采用界面聚合制备微胶囊相变材料。采用差示扫描量热仪(DSC)、扫描电镜(SEM)、光学显微镜等分别对微胶囊的热性能、表面形态进行研究和分析。所制备微胶囊表面光滑致密,相变温度24.2℃,相变热90 J/g。对微胶囊的致密性和稳定性研究结果表明,所制备丙三醇改性微胶囊的致密性和稳定性,如耐乙醇洗涤稳定性和耐热稳定性均比传统的未改性微胶囊有很大程度的提高。%Glycerol modified polyurea microcapsules containing butyl stearate as phase change material (PCM) was successfully synthesized by interracial polycondensation of toluene-2,4-diimcyanate (TDI) and diethylene triarnine (DETA). Styrene maleic anhydride copolymer (SMA) was used as emulsifier. The thermal properties, surface morphologies of microcapsules were investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron microscope (SEM) and optical microscope, respectively. The results indicate that the surface of the prepared microencapsulated phase change materials (microPCMs) is smooth and compact and have an phase change temperature of 24.2 ℃ and phase change heat of 90 J/g. The compactness and stabilities of microcapsules were aim investigated, the results indicate that the compactness and stabilities of the glycerol modified microcapsule, such as anti-ethanol wash and anti-heat properties are obiously improved than that of non modified microcapsule.

  9. Critical evaluation of methodology commonly used in sample collection, storage and preparation for the analysis of pharmaceuticals and illicit drugs in surface water and wastewater by solid phase extraction and liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Baker, David R; Kasprzyk-Hordern, Barbara

    2011-11-04

    The main aim of this manuscript is to provide a comprehensive and critical verification of methodology commonly used for sample collection, storage and preparation in studies concerning the analysis of pharmaceuticals and illicit drugs in aqueous environmental samples with the usage of SPE-LC/MS techniques. This manuscript reports the results of investigations into several sample preparation parameters that to the authors' knowledge have not been reported or have received very little attention. This includes: (i) effect of evaporation temperature and (ii) solvent with regards to solid phase extraction (SPE) extracts; (iii) effect of silanising glassware; (iv) recovery of analytes during vacuum filtration through glass fibre filters and (v) pre LC-MS filter membranes. All of these parameters are vital to develop efficient and reliable extraction techniques; an essential factor given that target drug residues are often present in the aqueous environment at ng L(-1) levels. Presented is also the first comprehensive review of the stability of illicit drugs and pharmaceuticals in wastewater. Among the parameters studied are: time of storage, temperature and pH. Over 60 analytes were targeted including stimulants, opioid and morphine derivatives, benzodiazepines, antidepressants, dissociative anaesthetics, drug precursors, human urine indicators and their metabolites. The lack of stability of analytes in raw wastewater was found to be significant for many compounds. For instance, 34% of compounds studied reported a stability change >15% after only 12 h in raw wastewater stored at 2 °C; a very important finding given that wastewater is typically collected with the use of 24 h composite samplers. The stability of these compounds is also critical given the recent development of so-called 'sewage forensics' or 'sewage epidemiology' in which concentrations of target drug residues in wastewater are used to back-calculate drug consumption. Without an understanding of stability

  10. Separation and analysis of phenolic acids from Salvia miltiorrhiza and its related preparations by off-line two-dimensional hydrophilic interaction chromatography×reversed-phase liquid chromatography coupled with ion trap time-of-flight mass spectrometry.

    Science.gov (United States)

    Sun, Wanyang; Tong, Ling; Miao, Jingzhuo; Huang, Jingyi; Li, Dongxiang; Li, Yunfei; Xiao, Hongting; Sun, Henry; Bi, Kaishun

    2016-01-29

    Salvia miltiorrhiza (SM) is one of the most widely used Traditional Chinese Medicine. Active constituents of SM mainly contain hydrophilic phenolic acids (PAs) and lipophilic tanshinones. However, due to the existing of multiple ester bonds and unsaturated bonds in the structures, PAs have numerous chemical conversion products. Many of them are so low-abundant that hard to be separated using conventional methods. In this study, an off-line two-dimensional liquid chromatography (2D-LC) method was developed to separate PAs in SM and its related preparations. In the first dimension, samples were fractionated by hydrophilic interaction chromatography (HILIC) (Acchrom×Amide, 4.6×250mm, 5μm) mainly based on the hydrogen bonding effects. The fractions were then separated on reversed-phase liquid chromatography (RP-LC) (Acquity HSS T3, 2.1×50mm, 1.7μm) according to hydrophobicity. For the selective identification of PAs, diode array detector (DAD) and electrospray ionization tandem ion trap time-of-flight mass spectrometry (ESI-IT-TOF-MS) were employed. Practical and effective peak capacities of all the samples were greater than 2046 and 1130, respectively, with the orthogonalities ranged from 69.7% to 92.8%, which indicated the high efficiency and versatility of this method. By utilizing the data post-processing techniques, including mass defect filter, neutral loss filter and product ion filter, a total of 265 compounds comprising 196 potentially new PAs were tentatively characterized. Twelve kinds of derivatives, mainly including glycosylated compounds, O-alkylated compounds, condensed compounds and hydrolyzed compounds, constituted the novelty of the newly identified PAs. The HILIC×RP-LC/TOF-MS system expanded our understanding on PAs of S. miltiorrhiza and its related preparations, which could also benefit the separation and characterization of polar constituents in complicated herbal extracts. Copyright © 2016. Published by Elsevier B.V.

  11. Sample preparation

    International Nuclear Information System (INIS)

    Anon.

    1992-01-01

    Sample preparation prior to HPLC analysis is certainly one of the most important steps to consider in trace or ultratrace analysis. For many years scientists have tried to simplify the sample preparation process. It is rarely possible to inject a neat liquid sample or a sample where preparation may not be any more complex than dissolution of the sample in a given solvent. The last process alone can remove insoluble materials, which is especially helpful with the samples in complex matrices if other interactions do not affect extraction. Here, it is very likely a large number of components will not dissolve and are, therefore, eliminated by a simple filtration process. In most cases, the process of sample preparation is not as simple as dissolution of the component interest. At times, enrichment is necessary, that is, the component of interest is present in very large volume or mass of material. It needs to be concentrated in some manner so a small volume of the concentrated or enriched sample can be injected into HPLC. 88 refs

  12. Representing culture in interstellar messages

    Science.gov (United States)

    Vakoch, Douglas A.

    2008-09-01

    As scholars involved with the Search for Extraterrestrial Intelligence (SETI) have contemplated how we might portray humankind in any messages sent to civilizations beyond Earth, one of the challenges they face is adequately representing the diversity of human cultures. For example, in a 2003 workshop in Paris sponsored by the SETI Institute, the International Academy of Astronautics (IAA) SETI Permanent Study Group, the International Society for the Arts, Sciences and Technology (ISAST), and the John Templeton Foundation, a varied group of artists, scientists, and scholars from the humanities considered how to encode notions of altruism in interstellar messages . Though the group represented 10 countries, most were from Europe and North America, leading to the group's recommendation that subsequent discussions on the topic should include more globally representative perspectives. As a result, the IAA Study Group on Interstellar Message Construction and the SETI Institute sponsored a follow-up workshop in Santa Fe, New Mexico, USA in February 2005. The Santa Fe workshop brought together scholars from a range of disciplines including anthropology, archaeology, chemistry, communication science, philosophy, and psychology. Participants included scholars familiar with interstellar message design as well as specialists in cross-cultural research who had participated in the Symposium on Altruism in Cross-cultural Perspective, held just prior to the workshop during the annual conference of the Society for Cross-cultural Research . The workshop included discussion of how cultural understandings of altruism can complement and critique the more biologically based models of altruism proposed for interstellar messages at the 2003 Paris workshop. This paper, written by the chair of both the Paris and Santa Fe workshops, will explore the challenges of communicating concepts of altruism that draw on both biological and cultural models.

  13. Semantic Representatives of the Concept

    Directory of Open Access Journals (Sweden)

    Elena N. Tsay

    2013-01-01

    Full Text Available In the article concept as one of the principle notions of cognitive linguistics is investigated. Considering concept as culture phenomenon, having language realization and ethnocultural peculiarities, the description of the concept “happiness” is presented. Lexical and semantic paradigm of the concept of happiness correlates with a great number of lexical and semantic variants. In the work semantic representatives of the concept of happiness, covering supreme spiritual values are revealed and semantic interpretation of their functioning in the Biblical discourse is given.

  14. [Determination of metformin hydrochloride, melamine and dicyandiamide in metformin hydrochloride preparations by tandem dual solid phase extraction cartridges-high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry].

    Science.gov (United States)

    Zhou, Yanfen; Wang, Fanghuan; Wang, Zelan; Zhan, Haijuan; Liu, Wanyi; Meng, Zhe

    2018-02-08

    A method for the confirmation and quantification of metformin hydrochloride and its relative substances melamine and dicyandiamide using tandem dual solid phase extraction (SPE) cartridges and high performance liquid chromatography-electrospray ionization multi-stage mass spectrometry (HPLC-ESI-MS n ) was developed. The samples were extracted with anhydrous ethanol containing 0.1% (v/v) acetic acid under ultrasound-assisted conditions. The extracts were concentrated and purified using Cleanert PCX and C18 tandem dual solid phase extraction cartridges, and eluted with 5% (v/v) ammonia methanol solution. The separation was performed on a Kromasil-C18 column (100 mm×4.6 mm, 3.5 μm) with gradient elution. The detection was performed in selected ion monitoring (SIM) mode using electrospray ionization multi-stage mass spectrometry. The external standard method was used for quantification. The extraction solvents, types of SPE cartridges and eluents were optimized by comparing the recoveries under different conditions. The results showed that the detector response of each target compound was linear in corresponding mass concentration ranges with the correlation coefficients ( r 2 ) ≥ 0.9992. The limits of detection (LODs) and the limits of quantification (LOQs) of the three analytes were 1.48-13.61 μg/kg and 5.96-45.67 μg/kg, respectively. The recoveries of the three analytes were 65.02%-118.33% spiked at low, medium and high levels. The relative standard deviations (RSDs) were no more than 13.41%. The method is reliable, easy, and has a better purification effect. The method can be applied to the routine analysis of metformin hydrochloride and its relative substances melamine and dicyandiamide in different preparations of metformin hydrochloride.

  15. Bowel preparation for CT colonography

    International Nuclear Information System (INIS)

    Neri, Emanuele; Lefere, Philippe; Gryspeerdt, Stefaan; Bemi, Pietro; Mantarro, Annalisa; Bartolozzi, Carlo

    2013-01-01

    Bowel preparation represents an essential part of CT colonography, as the accuracy of the exam is strongly related to the adequacy of colonic cleansing, and a poor bowel preparation may compromise the diagnostic quality even despite optimization of all other acquisition parameters. Residual stool and fluid in the large bowel may affect the interpretation of the exam and may increase the number of false positives and false negatives. In this regard, the majority of patients having undergone CT colonography state that bowel preparation is the most unpleasant part. Unfortunately, to date no definite consensus has been reached about the ideal bowel preparation technique, and there is great variability in preparation strategies across diagnostic centers. The purpose of this review article is to describe the development and evolution of bowel preparation techniques in order to choose the best approach for optimizing the diagnostic quality of CT colonography in each patient

  16. Bowel preparation for CT colonography

    Energy Technology Data Exchange (ETDEWEB)

    Neri, Emanuele, E-mail: emanuele.neri@med.unipi.it [Diagnostic and Interventional Radiology, University of Pisa (Italy); Lefere, Philippe; Gryspeerdt, Stefaan [Department of Radiology, Stedelijk Ziekenhuis, Roeselare (Belgium); Bemi, Pietro; Mantarro, Annalisa; Bartolozzi, Carlo [Diagnostic and Interventional Radiology, University of Pisa (Italy)

    2013-08-15

    Bowel preparation represents an essential part of CT colonography, as the accuracy of the exam is strongly related to the adequacy of colonic cleansing, and a poor bowel preparation may compromise the diagnostic quality even despite optimization of all other acquisition parameters. Residual stool and fluid in the large bowel may affect the interpretation of the exam and may increase the number of false positives and false negatives. In this regard, the majority of patients having undergone CT colonography state that bowel preparation is the most unpleasant part. Unfortunately, to date no definite consensus has been reached about the ideal bowel preparation technique, and there is great variability in preparation strategies across diagnostic centers. The purpose of this review article is to describe the development and evolution of bowel preparation techniques in order to choose the best approach for optimizing the diagnostic quality of CT colonography in each patient.

  17. Conspicuous Waste and Representativeness Heuristic

    Directory of Open Access Journals (Sweden)

    Tatiana M. Shishkina

    2017-12-01

    Full Text Available The article deals with the similarities between conspicuous waste and representativeness heuristic. The conspicuous waste is analyzed according to the classic Veblen’ interpretation as a strategy to increase social status through conspicuous consumption and conspicuous leisure. In “The Theory of the Leisure Class” Veblen introduced two different types of utility – conspicuous and functional. The article focuses on the possible benefits of the analysis of conspicuous utility not only in terms of institutional economic theory, but also in terms of behavioral economics. To this end, the representativeness heuristics is considered, on the one hand, as a way to optimize the decision-making process, which allows to examine it in comparison with procedural rationality by Simon. On the other hand, it is also analyzed as cognitive bias within the Kahneman and Twersky’ approach. The article provides the analysis of the patterns in the deviations from the rational behavior strategy that could be observed in case of conspicuous waste both in modern market economies in the form of conspicuous consumption and in archaic economies in the form of gift-exchange. The article also focuses on the marketing strategies for luxury consumption’ advertisement. It highlights the impact of the symbolic capital (in Bourdieu’ interpretation on the social and symbolic payments that actors get from the act of conspicuous waste. This allows to perform a analysis of conspicuous consumption both as a rational way to get the particular kind of payments, and, at the same time, as a form of institutionalized cognitive bias.

  18. Electrochemical preparation of new uranium oxide phases

    International Nuclear Information System (INIS)

    Smolenskij, V.V.; Lyalyushkin, N.V.; Bove, A.L.; Komarov, V.K.; Kapshukov, I.I.

    1992-01-01

    Behaviour of uranium ions in oxidation states 3+ and 4+ in molten chlorides of alkali metals in the temperature range of 700-900 degC in the atmosphere of an inert gas was studied by the method of cyclic voltametry. It is shown that as a result of introduction of crystal uranium dioxide into the salt melt formation of uranium oxide ions of the composition UO + and UO 2+ occurs, the ions participating in electrode reactions and bringing about formation of the following uranium oxides on the cathode: UO and, presumably, U 3 O 4 . Oxides UO and U 3 O 4 are thermodynamically unstable at low temperatures and decompose into uranium oxide of the composition UO 2-x , where x varies from 0 to 0.05, and metal uranium

  19. Administrative activities in the phase of preparation

    International Nuclear Information System (INIS)

    Guenther, J.A.

    1975-01-01

    Details of the licensing procedure in the FRG: site selection, necessary documents for application, selection of a safety level for the plant in question, organization of the licensing authority, consultant and expert activities. (HP) [de

  20. Facile preparation of surface-exchangeable core@shell iron oxide@gold nanoparticles for magnetic solid-phase extraction: Use of gold shell as the intermediate platform for versatile adsorbents with varying self-assembled monolayers

    Energy Technology Data Exchange (ETDEWEB)

    Li, Yaping [Beijing National Laboratory of Molecular Sciences, Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Graduate School, University of Chinese Academy of Sciences, Beijing 100049 (China); Qi, Li, E-mail: qili@iccas.ac.cn [Beijing National Laboratory of Molecular Sciences, Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Shen, Ying [Beijing National Laboratory of Molecular Sciences, Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China); Graduate School, University of Chinese Academy of Sciences, Beijing 100049 (China); Ma, Huimin [Beijing National Laboratory of Molecular Sciences, Key Laboratory of Analytical Chemistry for Living Biosystems, Institute of Chemistry, Chinese Academy of Sciences, Beijing 100190 (China)

    2014-02-06

    Graphical abstract: -- Highlights: •The core@shell Fe{sub 3}O{sub 4}@Au nanoparticles functionalized with SAMs were successfully constructed. •The SAMs could be transformed from one kind to another via thiol exchange process. •The developed nanomaterials could be applied in mode switching MSPE. -- Abstract: The core@shell Fe{sub 3}O{sub 4}@Au nanoparticles (NPs) functionalized with exchangeable self-assembled monolayers have been developed for mode switching magnetic solid-phase extraction (MSPE) using high performance liquid chromatography with ultraviolet detection. The adsorbents were synthesized by chemical coprecipitation to prepare magnetic cores followed by sonolysis to produce gold shells. Functionalization of Fe{sub 3}O{sub 4}@Au NPs surface was realized through self-assembly of commercially available low molecular weight thiol-containing ligands using gold shells as intermediate platform and the dynamic nature of Au–S chemistry allowed substituent of one thiol-containing ligand with another simply by thiol exchange process. The resultant adsorbents were characterized by transmission electronic microscopy, Fourier transform infrared spectroscopy, elemental analysis, contact angle measurement, and vibrating sample magnetometry. To evaluate the versatile performance of the developed MSPE adsorbents, they were applied for normal-phase SPE followed by reversed-phase SPE. A few kinds of diphenols and polycyclic aromatic hydrocarbons (PAHs) were employed as model analytes, respectively. The predominant parameters affecting extraction efficiency were investigated and optimized. Under the optimum experimental conditions, wide dynamic linear range (6.25–1600 μg L{sup −1} for diphenols and 1.56–100 μg L{sup −1} for PAHs) with good linearity (r{sup 2} ≥ 0.989) and low detection limits (0.34–16.67 μg L{sup −1} for diphenols and 0.26–0.52 μg L{sup −1} for PAHs) were achieved. The advantage of the developed method is that the Fe{sub 3}O

  1. Thermal behavior and phase transformation of ZrO{sub 2}–10%SiO{sub 2} precursor powder prepared by a co-precipitation route without adding stability agent

    Energy Technology Data Exchange (ETDEWEB)

    Chu, Hsueh-Liang [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Hwang, Weng-Sing [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Institute of Nanotechnology and Microsystems Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, Cheng-Li [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, Moo-Chin, E-mail: mcwang@kmu.edu.tw [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Lee, Kuen-Chan [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 80708, Taiwan (China); Huang, Hong-Hsin [Department of Electrical Engineering, Cheng Shiu University, 840 Cheng Ching Road, Niaosong, Kaohsiung 83347, Taiwan (China); Lee, Huey-Er, E-mail: huerle@kmu.edu.tw [School of Dentistry, College of Dental Medicine, Kaohsiung Medical University, 100 Shih-Chuan 1st Road, Kaohsiung 807, Taiwan (China); Department of Dentistry, Kaohsiung Medical University, 100 Tzyou 1st Road, Kaohsiung 807, Taiwan (China)

    2014-12-15

    Highlights: • The precursor powders contained about 68.3 wt% ZrO{sub 2}, which corresponds to ZrO{sub 2}·1/8 H{sub 2}O. • The exothermic peak temperature of tetragonal ZrO{sub 2} formation occurred at 1014 K. • The activation energy of ZrO{sub 2}–10%SiO{sub 2} precursors crystallization is 993.7 kJ/mol. • Only the tetragonal ZrO{sub 2} formed when the precursor calcined at 1173–1373 K for 2 h. • As calcined at 1473 K for 2 h, tetragonal ZrO{sub 2} fully converted to monoclinic ZrO{sub 2}. - Abstract: Thermal behavior and phase transformation of ZrO{sub 2}–10%SiO{sub 2} precursor powder prepared by a co-precipitation route without adding stability agent has been studied using different thermal analysis/thermogravimetry (DTA/TG), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), nano beam electron diffraction (NBED), high-resolution TEM (HRTEM) and energy-dispersive X-ray spectrometer (EDS). The TG results show that four weight loss regions were from 298 to 443 K, 443 to 743 K, 743 to 793 K and 793 to 1400 K. The DTA result shows that the ZrO{sub 2} freeze-dried precursor powders crystallization at 1014 K. The activation energy of 993.7 kJ/mol was obtained for tetragonal ZrO{sub 2} crystallization using a non-isothermal process. The XRD result shows that only a single phase of tetragonal ZrO{sub 2} appears when the freeze-dried precursor powders after calcination between 1173 and 1373 K for 2 h. Moreover, when calcined at 1473 K for 2 h, the phase transformation from tetragonal ZrO{sub 2} fully converted to monoclinic ZrO{sub 2} occurred.

  2. Modified Activated Carbon Prepared from Acorn Shells as a New Solid-Phase Extraction Sorbent for the Preconcentration and Determination of Trace Amounts of Nickel in Food Samples Prior to Flame Atomic Absorption Spectrometry.

    Science.gov (United States)

    Ebrahimi, Bahram

    2017-03-01

    A new solid-phase extraction (SPE) sorbent was introduced based on acidic-modified (AM) activated carbon (AC) prepared from acorn shells of native oak trees in Kurdistan. Hydrochloric acid (15%, w/w) and nitric acid (32.5%, w/w) were used to condition and modify AC. The IR spectra of AC and AM-AC showed that AM lead to the formation of increasing numbers of acidic functional groups on AM-AC. AM-AC was used in the SPE method for the extraction and preconcentration of Ni+2 prior to flame atomic absorption spectrometric determination at ng/mL levels in model and real food samples. Effective parameters of the SPE procedure, such as the pH of the solutions, sorbent dosage, extraction time, sample volume, type of eluent, and matrix ions, were considered and optimized. An enrichment factor of 140 was obtained. The calibration curve was linear with an R2 of 0.997 in the concentration range of 1-220 ng/mL. The RSD was 5.67% (for n = 7), the LOD was 0.352 ng/mL, and relative recoveries in vegetable samples ranged from 96.7 to 103.7%.

  3. From deposit modelling to the mine plan engineering guidance in a Greenfield project for the opening of a lignite open-cast mine during the preparation and development phase

    International Nuclear Information System (INIS)

    Hertling, H.

    2010-01-01

    In order to supply the nearby power plant Elbistan B, a new open-cast mine is being developed at the Collolar Field in Turkey. Initial fieldwork began in mid-2007, followed by overburden removal in early 2008 and lignite production in 2009. Several planning studies have been undertaken in order to prepare and undertake the initial work in just under two years, including the establishment of a geological model as a basis for calculating reserves, and for hydrological and geotechnical calculations, leading to a drainage concept and the formulation of requirements made on the slope stability. This paper presented the framework concept for the modelling and discussed the geological modelling and selection of a suitable development plan. The hydrological calculations and planning of drainage measures were also outlined. The more detailed plans for phase two, including the database for hydro-geological modelling, pumping tests and laboratory tests, ground water modelling, and the dewatering concept were also presented. The paper also discussed the determination of geotechnical parameters, calculation methods, and the slope stabilities at the mining and dumping site. It was concluded that regular comparison to plans and calculations on drainage and slope stability must be conducted when planning and operating a mine. 3 figs.

  4. Representative mass reduction in sampling

    DEFF Research Database (Denmark)

    Petersen, Lars; Esbensen, Harry Kim; Dahl, Casper Kierulf

    2004-01-01

    We here present a comprehensive survey of current mass reduction principles and hardware available in the current market. We conduct a rigorous comparison study of the performance of 17 field and/or laboratory instruments or methods which are quantitatively characterized (and ranked) for accuracy...... dividers, the Boerner Divider, the ??spoon method??, alternate/fractional shoveling and grab sampling. Only devices based on riffle splitting principles (static or rotational) passes the ultimate representativity test (with minor, but significant relative differences). Grab sampling, the overwhelmingly...... most often used mass reduction method, performs appallingly?its use must be discontinued (with the singular exception for completely homogenized fine powders). Only proper mass reduction (i.e. carried out in complete compliance with all appropriate design principles, maintenance and cleaning rules) can...

  5. 十八烷/聚(St-MMA)相变微胶囊制备及表征%Preparation and Characterization of n-Octadecane/P(St-MMA) Phase-change Microcapsules

    Institute of Scientific and Technical Information of China (English)

    武卫莉; 李江坤

    2017-01-01

    采用乳液聚合的方法,分别选取聚苯乙烯(PS)、聚甲基丙烯酸甲酯(PMMA)或苯乙烯和甲基丙烯酸甲酯的共聚物为壁材,正十八烷为芯材,十二烷基苯磺酸钠(SDBS)为乳化剂,制作相变储能微胶囊.用粒径分析仪、透射电子显微镜(TEM)、热重分析仪(TG)和示差扫描量热测试仪(DSC)对微胶囊的形貌、相变热性能和热稳定性分别进行表征.结果表明:壁材选取两者共聚物,当两种单体的比例为St∶ MMA=1∶5,SDBS用量为1.5g(总质量的3%)时,微胶囊粒径大小均匀,粒子分散性好,壁材的包裹性好.微胶囊的放热峰为起始温度为27.3℃,终止温度为31.9℃,相变温度为28.9℃,相变焓为48.4J/g.TG表明长期使用温度不能超过131℃.IR分析微胶囊中含有芯材和壁材.这种十八烷/聚(St-MMA)相变微胶囊可以用于诸能材料.%A phase-change stored energy microcapsules were prepared by polymerization,in which polystyrene (PS),poly methyl methacrylate (PMMA) or copolymers of styrene and methyl methacrylate were used as shell materials,n-octadecane was used as a core material,and sodium dodecyl benzene sulfonate (SDBS) as a emulsifier.The morphology,phase-change thermal properties and thermal stability of microcapsules,respectively,were characterized by particle size analyzer,transmission electron microscope (TEM),thermogravimetric analyzer (TG) and differential scanning calorimetry (DSC).The results show that the particle size of microcapsules is uniform,the particle dispersion is good,and the shell is well wrapped when the copolymer of styrene (St) and methyl methacrylate (MMA),both mass ratio is 1∶5),is used as shell material,and sodium dodecyl benzene sulfonate content is 1.5g (3% of the total mass).The heat release peaks of microcapsules are at 27.3℃ of starting temperature,at 31.9℃ of end temperature,and the phase transformation temperature is 28.9℃,the phase-change enthalpy of microcapsules is 48.4J

  6. PSCAD Modules Representing PV Generator

    Energy Technology Data Exchange (ETDEWEB)

    Muljadi, E.; Singh, M.; Gevorgian, V.

    2013-08-01

    Photovoltaic power plants (PVPs) have been growing in size, and the installation time is very short. With the cost of photovoltaic (PV) panels dropping in recent years, it can be predicted that in the next 10 years the contribution of PVPs to the total number of renewable energy power plants will grow significantly. In this project, the National Renewable Energy Laboratory (NREL) developed a dynamic modeling of the modules to be used as building blocks to develop simulation models of single PV arrays, expanded to include Maximum Power Point Tracker (MPPT), expanded to include PV inverter, or expanded to cover an entire PVP. The focus of the investigation and complexity of the simulation determines the components that must be included in the simulation. The development of the PV inverter was covered in detail, including the control diagrams. Both the current-regulated voltage source inverter and the current-regulated current source inverter were developed in PSCAD. Various operations of the PV inverters were simulated under normal and abnormal conditions. Symmetrical and unsymmetrical faults were simulated, presented, and discussed. Both the three-phase analysis and the symmetrical component analysis were included to clarify the understanding of unsymmetrical faults. The dynamic model validation was based on the testing data provided by SCE. Testing was conducted at SCE with the focus on the grid interface behavior of the PV inverter under different faults and disturbances. The dynamic model validation covers both the symmetrical and unsymmetrical faults.

  7. Want change? Call your representative

    Science.gov (United States)

    Fischhoff, Ilya R.

    2011-07-01

    During my tenure as an AGU Congressional Science Fellow, which began in September 2010 and continues until November 2011, my time has been shared between working with the U.S. House of Representatives Natural Resource Committee Democratic staff and in the office of Rep. Ed Markey (D-Mass., ranking Democrat on the committee). I appreciate getting to work with staff, fellows, and interns who inspire me, make me laugh, and know their issues cold. Much of my work on the committee is related to fish, wildlife, oceans, lands, and water issues and is directly related to my background in ecology and evolutionary biology (I studied zebra ecology and behavior in Kenya). My assignments have included asking the Environmental Protection Agency (EPA) about why it has not changed the allowed usage of certain pesticides that the National Marine Fisheries Service has found to jeopardize the recovery of endangered Pacific salmon; helping to identify research needs and management options to combat the swiftly spreading and catastrophic white nose syndrome in North American bats; and inquiring as to whether a captive-ape welfare bill, if passed without amendment, could thwart development of a vaccine to stop the Ebola virus from continuing to cause mass mortality in endangered wild apes.

  8. Radioprotective preparation

    International Nuclear Information System (INIS)

    Stefanova, D.; Frattadochi, A.; Gattavecchia, E.; Ferri, E.; Tonnelli, D.

    1988-01-01

    The invention is intended for radiation injuries prophylaxis in mammals. It has an well expressed radioprotective effect against acute gamma irradiation on cellular level as well as a prolonged action when applied up to 48 hours before the acute irradiation. The preparation is a coprecipitate of the natural tripeptide glutathione (reduced form) and polyvinyl pyrrolidone (pvp) in ratio 30-60/70-40. It is obtained by incubation method with subsequent lyophilization from water solution of the initial components. The molecular mass of the pvp is 20 till 360.10 3 . 2 claims

  9. Target preparation

    International Nuclear Information System (INIS)

    Hinn, G.M.

    1984-01-01

    A few of the more interesting of the 210 targets prepared in the Laboratory last year are listed. In addition the author continues to use powdered silver mixed with /sup 9,10/BeO to produce sources for accelerator radio dating of Alaskan and South Polar snow. Currently, he is trying to increase production by multiple sample processing. Also the author routinely makes 3 μg/cm 2 cracked slacked carbon stripper foils and is continuing research with some degree of success in making enriched 28 Si targets starting with the oxide

  10. Influence of foaming agents on solid thermal conductivity of foam glasses prepared from CRT panel glass

    DEFF Research Database (Denmark)

    Østergaard, Martin Bonderup; Petersen, Rasmus Rosenlund; König, Jakob

    2017-01-01

    The understanding of the thermal transport mechanism of foam glass is still lacking. The contribution of solid- and gas conduction to the total thermal conductivity remains to be reported. In many foam glasses, the solid phase consist of a mix of an amorphous and a crystalline part where foaming...... containing glass and crystalline foaming agents and amorphous samples where the foaming agents are completely dissolved in the glass structure, respectively. Results show that the samples prepared by sintering have a higher thermal conductivity than the samples prepared by melt-quenching. The thermal...... conductivities of the sintered and the melt-quenched samples represent an upper and lower limit of the solid phase thermal conductivity of foam glasses prepared with these foaming agents. The content of foaming agents dissolved in the glass structure has a major impact on the solid thermal conductivity of foam...

  11. Characterization and study of reduction and sulfurization processing in phase transition from molybdenum oxide (MoO{sub 2}) to molybdenum disulfide (MoS{sub 2}) chalcogenide semiconductor nanoparticles prepared by one-stage chemical reduction method

    Energy Technology Data Exchange (ETDEWEB)

    Shomalian, K.; Bagheri-Mohagheghi, M.M.; Ardyanian, M. [Damghan University, School of Physics, Damghan (Iran, Islamic Republic of)

    2017-01-15

    In this research, molybdenum disulfide (MoS{sub 2}) nanoparticles were prepared by chemical reduction method using MoO{sub 3} and thiourea as a precursor. The physical properties of the synthesized MoO{sub 2}-MoS{sub 2} nanoparticles annealed at different temperatures of 200, 300, 750 C have been investigated, before and after exposure to sulfur vapor. The nanostructure of nanoparticles has been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM) analyses and UV-Vis spectrophotometer. The X-ray diffraction analysis showed the formation of MoS{sub 2} single phase at annealing temperature of 750 C in the presence of sulfur vapor. The Raman spectrum of the nanoparticles revealed that the formation of MoS{sub 2} at 750 C after annealing in sulfur vapor. The values of band gap were obtained in the range of 3.64-3.17 eV and 3.47-1.95 eV for MoS{sub 2} nanoparticles before and after exposure to sulfur vapor, respectively. According to SEM images, the grain size decreases with increasing annealing temperature up to 750 C. Also, nanoplate-nanoparticles of MoS{sub 2} are formed at annealing temperature of 200-750 C. The TEM images of MoS{sub 2} nanoparticles at T{sub a} = 750 C confirm that the nanoparticles have a homogeneous distribution with a hexagonal structure. The FTIR spectra of the MoS{sub 2} nanoparticles showed the peaks at about 467 cm {sup -1} belong to the characteristic bands of Mo-S. (orig.)

  12. Preparation of magnetic graphene/mesoporous silica composites with phenyl-functionalized pore-walls as the restricted access matrix solid phase extraction adsorbent for the rapid extraction of parabens from water-based skin toners.

    Science.gov (United States)

    Feng, Jianan; He, Xinying; Liu, Xiaodan; Sun, Xueni; Li, Yan

    2016-09-23

    In this work, phenyl-functionalized magnetic graphene/mesoporous silica composites (MG-mSiO2-Ph) were prepared and applied as restricted access matrix solid phase extraction (RAM-SPE) adsorbents to determine the parabens in commercially available retail cosmetics. MG-mSiO2-Ph composites were synthesized by a surfactant-mediated co-condensation reaction in which mesoporous silica with phenyl-functionalized pore-walls was coated on a magnetic graphene sheet. The obtained nano-composites were proven to be of sufficient quality for an ideal RAM-SPE adsorbent with a large specific surface area of 369m(2)g(-1), uniform mesopores of 2.8nm, and special phenyl-functionalized pore-walls. Parabens, such as methyl paraben, ethyl paraben and propyl paraben, were extracted from water-based skin toners using one step of the RAM-SPE and were then analysed by a HPLC-DAD system. The SPE conditions were optimized by studying the parameters, such as the adsorbent amount, elution solvent type, adsorption time and desorption time, that influence the extraction efficiency. For each analyte, there were good linearities of approximately 0.10-120μgmL(-1) with determination coefficients (R(2))>0.995. The sensitivity was as low as 0.01-0.025μgmL(-1) for the LOD, and the percent recoveries were 98.37-105.84%. The intra-day and inter-day RSDs were 1.44-6.11% (n=6) and 3.12-11.70% (n=6), respectively. The results indicated that this method with novel RAM-SPE adsorbents is sensitive and convenient. The results also offered an attractive alternative for the extraction and determination of paraben preservatives in a complex matrix, such as cosmetics. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. PREPARATION AND CHARACTERIZATION OF DIALDEHYDE ...

    African Journals Online (AJOL)

    User

    Dialdehyde starch urea (DASU) was prepared by the reaction of dialdehyde starch (DAS) from ... is representative one for the treatment of heavy metal ... It was reported that Potassium ... 0.2mol/L sulfuric acid, 100cm3 of water and 2cm3 of.

  14. Beneficial effects of a Fermented Papaya Preparation for the treatment of electrohypersensitivityself-reporting patients: results of a phaseI-IIclinicaltrialwith special reference to cerebral pulsationmeasurement and oxidative stress analysis

    Directory of Open Access Journals (Sweden)

    Irigaray Philippe

    2018-02-01

    Full Text Available Background: Electromagnetic Field Intolerance Syndrome (EMFIS, also termed Idiopathic Environmental Intolerance (IEI attributed to Electromagnetic Fields (IEI-EMF by WHO, is a newly identified pathological disorder occurring in electrohypersensitivity (EHS self-reporting patients. To date, there has been no recognized treatment of this disorder. We have shown that EHS self-reporting patients experience some degree of oxidative stress, inflammation, and autoimmune response. Additionally, Fermented Papaya Preparation (FPP has some antioxidant, anti-inflammation, and immuno-modulating properties. The objective of this phase I-II clinical trial was thus to test whether FPP treatment is well tolerated, can improve clinical outcomes, and normalize biological abnormalities. Methods: 32 EMFIS-bearing patients were serially included in this trial, among which 26 and 16 of them were evaluable after 3 and 6 months of FPP treatment, respectively. Clinical assessment was conducted during a specific face to face interview by using a validated pre-established questionnaire. Biological assessment consisted of measuring intracerebral tissue pulsometric index (PI in the temporal lobes with ultrasonic cerebral tomosphygmography (UCTS, in addition to oxidative stress and inflammation with a battery of oxidative stress and inflammation-related peripheral blood tests. Results: Overall clinical improvement was obtained in 50-60% of the cases, among which 20-35% presented major improvement that mainly consisted of the regression of cognitive symptoms such as loss of short term memory, concentration, attention deficiencies, insomnia, and fatigue. This clinical improvement was objectively supported by a statistically significant normal recovery of mean PI in the temporal lobes and by a FPP-related antioxidative effect evidenced by a statistically significant decrease in malondialdehyde levels in the plasma (p<0.0001 and increase in the Glutathione peroxidase activity in

  15. Characterization of Microemulsions Prepared using Isopropyl ...

    African Journals Online (AJOL)

    HP

    subjected to further characterization by polarized light microscopy, differential scanning calorimetry. (DSC) ... preparation and phase inversion. The aim .... propanol, D = butanol, E = pentanol .... and water-soluble compounds in triglycerides. In.

  16. An improved calcium chloride method preparation and ...

    African Journals Online (AJOL)

    Jane

    2010-12-13

    Dec 13, 2010 ... In this paper, we have reported a modified method for preparation and transformation of competent cells. This modified ... MATERIALS AND METHODS. Growth media ..... lipidic phase-transition temperature, and thus enhance.

  17. Using lean principles to improve outpatient adult infusion clinic chemotherapy preparation turnaround times.

    Science.gov (United States)

    Lamm, Matthew H; Eckel, Stephen; Daniels, Rowell; Amerine, Lindsey B

    2015-07-01

    The workflow and chemotherapy preparation turnaround times at an adult infusion clinic were evaluated to identify opportunities to optimize workflow and efficiency. A three-phase study using Lean Six Sigma methodology was conducted. In phase 1, chemotherapy turnaround times in the adult infusion clinic were examined one year after the interim goal of a 45-minute turnaround time was established. Phase 2 implemented various experiments including a five-day Kaizen event, using lean principles in an effort to decrease chemotherapy preparation turnaround times in a controlled setting. Phase 3 included the implementation of process-improvement strategies identified during the Kaizen event, coupled with a final refinement of operational processes. In phase 1, the mean turnaround time for all chemotherapy preparations decreased from 60 to 44 minutes, and a mean of 52 orders for adult outpatient chemotherapy infusions was received each day. After installing new processes, the mean turnaround time had improved to 37 minutes for each chemotherapy preparation in phase 2. In phase 3, the mean turnaround time decreased from 37 to 26 minutes. The overall mean turnaround time was reduced by 26 minutes, representing a 57% decrease in turnaround times in 19 months through the elimination of waste and the implementation of lean principles. This reduction was accomplished through increased efficiencies in the workplace, with no addition of human resources. Implementation of Lean Six Sigma principles improved workflow and efficiency at an adult infusion clinic and reduced the overall chemotherapy turnaround times from 60 to 26 minutes. Copyright © 2015 by the American Society of Health-System Pharmacists, Inc. All rights reserved.

  18. CrowdPhase: crowdsourcing the phase problem

    Energy Technology Data Exchange (ETDEWEB)

    Jorda, Julien; Sawaya, Michael R. [Institute for Genomics and Proteomics, 611 Charles Young Drive East, Los Angeles, CA 90095 (United States); Yeates, Todd O., E-mail: yeates@mbi.ucla.edu [Institute for Genomics and Proteomics, 611 Charles Young Drive East, Los Angeles, CA 90095 (United States); Molecular Biology Institute, 611 Charles Young Drive East, Los Angeles, CA 90095 (United States); University of California, 611 Charles Young Drive East, Los Angeles, CA 90095 (United States)

    2014-06-01

    The idea of attacking the phase problem by crowdsourcing is introduced. Using an interactive, multi-player, web-based system, participants work simultaneously to select phase sets that correspond to better electron-density maps in order to solve low-resolution phasing problems. The human mind innately excels at some complex tasks that are difficult to solve using computers alone. For complex problems amenable to parallelization, strategies can be developed to exploit human intelligence in a collective form: such approaches are sometimes referred to as ‘crowdsourcing’. Here, a first attempt at a crowdsourced approach for low-resolution ab initio phasing in macromolecular crystallography is proposed. A collaborative online game named CrowdPhase was designed, which relies on a human-powered genetic algorithm, where players control the selection mechanism during the evolutionary process. The algorithm starts from a population of ‘individuals’, each with a random genetic makeup, in this case a map prepared from a random set of phases, and tries to cause the population to evolve towards individuals with better phases based on Darwinian survival of the fittest. Players apply their pattern-recognition capabilities to evaluate the electron-density maps generated from these sets of phases and to select the fittest individuals. A user-friendly interface, a training stage and a competitive scoring system foster a network of well trained players who can guide the genetic algorithm towards better solutions from generation to generation via gameplay. CrowdPhase was applied to two synthetic low-resolution phasing puzzles and it was shown that players could successfully obtain phase sets in the 30° phase error range and corresponding molecular envelopes showing agreement with the low-resolution models. The successful preliminary studies suggest that with further development the crowdsourcing approach could fill a gap in current crystallographic methods by making it

  19. CrowdPhase: crowdsourcing the phase problem

    International Nuclear Information System (INIS)

    Jorda, Julien; Sawaya, Michael R.; Yeates, Todd O.

    2014-01-01

    The idea of attacking the phase problem by crowdsourcing is introduced. Using an interactive, multi-player, web-based system, participants work simultaneously to select phase sets that correspond to better electron-density maps in order to solve low-resolution phasing problems. The human mind innately excels at some complex tasks that are difficult to solve using computers alone. For complex problems amenable to parallelization, strategies can be developed to exploit human intelligence in a collective form: such approaches are sometimes referred to as ‘crowdsourcing’. Here, a first attempt at a crowdsourced approach for low-resolution ab initio phasing in macromolecular crystallography is proposed. A collaborative online game named CrowdPhase was designed, which relies on a human-powered genetic algorithm, where players control the selection mechanism during the evolutionary process. The algorithm starts from a population of ‘individuals’, each with a random genetic makeup, in this case a map prepared from a random set of phases, and tries to cause the population to evolve towards individuals with better phases based on Darwinian survival of the fittest. Players apply their pattern-recognition capabilities to evaluate the electron-density maps generated from these sets of phases and to select the fittest individuals. A user-friendly interface, a training stage and a competitive scoring system foster a network of well trained players who can guide the genetic algorithm towards better solutions from generation to generation via gameplay. CrowdPhase was applied to two synthetic low-resolution phasing puzzles and it was shown that players could successfully obtain phase sets in the 30° phase error range and corresponding molecular envelopes showing agreement with the low-resolution models. The successful preliminary studies suggest that with further development the crowdsourcing approach could fill a gap in current crystallographic methods by making it

  20. Liposomal preparations of muramyl glycopeptides as immunomodulators and adjuvants.

    Science.gov (United States)

    Turánek, Jaroslav; Ledvina, Miroslav; Kasná, Andrea; Vacek, Antonín; Hríbalova, Vera; Krejcí, Josef; Miller, Andrew D

    2006-04-12

    The need for safe and structurally defined immunomodulators and adjuvants is increasing in connection with the recently observed marked increase in the prevalence of pathological conditions characterized by immunodeficiency. Important groups of such compounds are muramyl glycopeptides, analogs of muramyl dipeptide (MDP), glucosaminyl-muramyl dipeptide (GMDP), and desmuramylpeptides. We have designed and synthesized new types of analogs with changes in both the sugar and the peptide parts of the molecule that show a high immunostimulating and adjuvant activity and suppressed adverse side effects. The introduction of lipophilic residues has also improved their incorporation into liposomes, which represent a suitable drug carrier. The proliposome-liposome method is based on the conversion of the initial proliposome preparation into liposome dispersion by dilution with the aqueous phase. The description of a home-made stirred thermostated cell and its link-up with a liquid delivery system for a rapid and automated preparation of multilamellar liposomes at strictly controlled conditions (sterility, temperature, dilution rate and schedule) is presented. The cell has been designed for laboratory-scale preparation of liposomes (300-1000 mg of phospholipid per run) in a procedure taking less than 90 min. The method can be readily scaled up. Examples of adjuvant and immunostimulatory effect of liposomal preparation in mice model will be presented.

  1. OAS :: Authorities : Permanent Representatives to the OAS

    Science.gov (United States)

    Rights Actions against Corruption C Children Civil Registry Civil Society Contact Us Culture Cyber Representative of Belize Diego Pary Rodríguez Bolivia Diego Pary Rodríguez Ambassador, Permanent Representative of Bolivia José Luiz Machado Brazil José Luiz Machado e Costa Ambassador, Permanent Representative

  2. Preparation and Characterization of Graphene

    Directory of Open Access Journals (Sweden)

    Xu Man

    2015-01-01

    Full Text Available The homogeneous-dispersed graphene oxide was prepared by the improved Hummers method, which would be reduced to graphene with the reducing agent called hydrazine hydrate. The X-ray diffraction, Infrared spectroscopy, Raman spectra and Transmission electron microscopy were used to analysis the phase, morphology and structure of the graphene and graphene oxide. The results show that the graphene oxide and reduced graphene oxide prepared via this method, whose degree of oxidation and reduction are high; Also obtained a higher well-disperses and less structural imperfection of the graphene that was manufactured in the reducing system that added ammonia reduction

  3. Preparing for faster filling

    CERN Multimedia

    CERN Bulletin

    2010-01-01

    Following the programmed technical stop last week, operators focussed on preparing the machine for faster filling, which includes multibunch injection and a faster pre-cycle phase.   The LHC1 screen shot during the first multibunch injection operation. The LHC operational schedule incorporates a technical stop for preventive maintenance roughly every six weeks of stable operation, during which several interventions on the various machines are carried out. Last week these included the replacement of a faulty magnet in the SPS pre-accelerator, which required the subsequent re-setting of the system of particle extraction and transfer to the LHC. At the end of last week, all the machines were handed back for operation and work could start on accommodating all the changes made into the complex systems in order for normal operation to be resumed. These ‘recovery’ operations continued through the weekend and into this week. At the beginning of this week, operators succeeded in pro...

  4. Preparing for Emergency Situations

    Science.gov (United States)

    Asproth, Viveca; Amcoff Nyström, Christina

    2010-11-01

    Disaster relief can be seen as a dynamic multi actor process with actors both joining and leaving the relief work during the help and rescue phase after the disaster has occurred. Actors may be governmental agencies, non profit voluntary organisations or spontaneous helpers comprised of individual citizens or temporal groups of citizens. Hence, they will vary widely in agility, competence, resources, and endurance. To prepare for for disasters a net based Agora with simulation of emergency situations for mutual preparation, training, and organisational learning is suggested. Such an Agora will ensure future security by: -Rising awareness and preparedness of potential disaster responders by help of the components and resources in the netAgora environment; -Improving cooperation and coordination between responders; -Improving competence and performance of organisations involved in security issues; -Bridging cultural differences between responders from different organizations and different backgrounds. The developed models are intended to reflect intelligent anticipatory systems for human operator anticipation of future consequences. As a way to catch what should be included in this netbased Agora and to join the split pictures that is present, Team Syntegrity could be a helpful tool. The purpose of Team Syntegrity is to stimulate collaboration and incite cross fertilization and creativity. The difference between syntegration and other group work is that the participants are evenly and uniquely distributed and will collectively have the means, the knowledge, the experience, the perspectives, and the expertise, to deal with the topic. In this paper the possibilities with using Team Syntegrity in preparation for the development of a netbased Agora is discussed. We have identified that Team Syntegrity could be useful in the steps User Integration, Designing the netAgora environment, developing Test Scenarios, and assessment of netAgora environment.

  5. β-Ga2O3 versus ε-Ga2O3: Control of the crystal phase composition of gallium oxide thin film prepared by metal-organic chemical vapor deposition

    Science.gov (United States)

    Zhuo, Yi; Chen, Zimin; Tu, Wenbin; Ma, Xuejin; Pei, Yanli; Wang, Gang

    2017-10-01

    Gallium oxide thin films of β and ε phase were grown on c-plane sapphire using metal-organic chemical vapor deposition and the phase compositions were analyzed using X-ray diffraction. The epitaxial phase diagram was constructed as a function of the growth temperature and VI/III ratio. A low growth temperature and low VI/III ratio were beneficial for the formation of hexagonal-type ε-Ga2O3. Further structure analysis revealed that the epitaxial relationship between ε-Ga2O3 and c-plane sapphire is ε-Ga2O3 (0001) || Al2O3 (0001) and ε-Ga2O3 || Al2O3 . The structural evolution of the mixed-phase sample during film thickening was investigated. By reducing the growth rate, the film evolved from a mixed phase to the energetically favored ε phase. Based on these results, a Ga2O3 thin film with a phase-pure ε-Ga2O3 upper layer was successfully obtained.

  6. Mechanism of formation of perovskite phase and dielectric properties of Pb(Zn,Mg)1/3Nb2/3O3 ceramics prepared by columbite precursor routes

    International Nuclear Information System (INIS)

    Jang, H.M.; Cho, S.R.; Lee, K.M.

    1995-01-01

    The mechanism of formation of the perovskite phase and the dielectric properties of Pb(Zn,Mg) 1/3 Nb 2/3 O 3 (PZMN) ceramics were examined using two different types of columbite precursors, (Mg,Zn)Nb 2 O 6 (MZN) and MgNb 2 O 6 + ZnNb 2 O 6 (MN + ZN). The formation of perovskite phase in the PbO + MN + ZN system is characterized by an initial rapid formation of Mg-rich perovskite phase, followed by a sluggish formation of Zn-rich perovskite phase. On the other hand, due to the formation of pyrochlore phase of mixed divalent cations Pb 2-x (Zn,Mg) y Nb 2-y O 7-x-3y/2 , the pyrochlore/perovskite transformation in the PbO + MZN system proceeded uniformly with a spatial homogeneity. Further analysis suggested that the formation of perovskite phase is a diffusion-controlled process. The degree of diffuseness of the rhombohedral/cubic phase transition (DPT) is higher in the PbO + MN + ZN system than in the PbO + MZN specimen for T > T max (temperature of the dielectric permittivity maximum), indicating a broadened compositional distribution of the B-site cations in the PbO + MN + ZN system

  7. Represented Speech in Qualitative Health Research

    DEFF Research Database (Denmark)

    Musaeus, Peter

    2017-01-01

    Represented speech refers to speech where we reference somebody. Represented speech is an important phenomenon in everyday conversation, health care communication, and qualitative research. This case will draw first from a case study on physicians’ workplace learning and second from a case study...... on nurses’ apprenticeship learning. The aim of the case is to guide the qualitative researcher to use own and others’ voices in the interview and to be sensitive to represented speech in everyday conversation. Moreover, reported speech matters to health professionals who aim to represent the voice...... of their patients. Qualitative researchers and students might learn to encourage interviewees to elaborate different voices or perspectives. Qualitative researchers working with natural speech might pay attention to how people talk and use represented speech. Finally, represented speech might be relevant...

  8. Preparing for Surgery

    Science.gov (United States)

    ... Events Advocacy For Patients About ACOG Preparing for Surgery Home For Patients Search FAQs Preparing for Surgery ... Surgery FAQ080, August 2011 PDF Format Preparing for Surgery Gynecologic Problems What is the difference between outpatient ...

  9. Sample preparation in foodomic analyses.

    Science.gov (United States)

    Martinović, Tamara; Šrajer Gajdošik, Martina; Josić, Djuro

    2018-04-16

    Representative sampling and adequate sample preparation are key factors for successful performance of further steps in foodomic analyses, as well as for correct data interpretation. Incorrect sampling and improper sample preparation can be sources of severe bias in foodomic analyses. It is well known that both wrong sampling and sample treatment cannot be corrected anymore. These, in the past frequently neglected facts, are now taken into consideration, and the progress in sampling and sample preparation in foodomics is reviewed here. We report the use of highly sophisticated instruments for both high-performance and high-throughput analyses, as well as miniaturization and the use of laboratory robotics in metabolomics, proteomics, peptidomics and genomics. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  10. Towards Representative Metallurgical Sampling and Gold Recovery Testwork Programmes

    Directory of Open Access Journals (Sweden)

    Simon C. Dominy

    2018-05-01

    Full Text Available When developing a process flowsheet, the risks in achieving positive financial outcomes are minimised by ensuring representative metallurgical samples and high quality testwork. The quality and type of samples used are as important as the testwork itself. The key characteristic required of any set of samples is that they represent a given domain and quantify its variability. There are those who think that stating a sample(s is representative makes it representative without justification. There is a need to consider both (1 in-situ and (2 testwork sub-sample representativity. Early ore/waste characterisation and domain definition are required, so that sampling and testwork protocols can be designed to suit the style of mineralisation in question. The Theory of Sampling (TOS provides an insight into the causes and magnitude of errors that may occur during the sampling of particulate materials (e.g., broken rock and is wholly applicable to metallurgical sampling. Quality assurance/quality control (QAQC is critical throughout all programmes. Metallurgical sampling and testwork should be fully integrated into geometallurgical studies. Traditional metallurgical testwork is critical for plant design and is an inherent part of geometallurgy. In a geometallurgical study, multiple spatially distributed small-scale tests are used as proxies for process parameters. These will be validated against traditional testwork results. This paper focusses on sampling and testwork for gold recovery determination. It aims to provide the reader with the background to move towards the design, implementation and reporting of representative and fit-for-purpose sampling and testwork programmes. While the paper does not intend to provide a definitive commentary, it critically assesses the hard-rock sampling methods used and their optimal collection and preparation. The need for representative sampling and quality testwork to avoid financial and intangible losses is

  11. Preparation of inorganic crystalline compounds induced by ionizing, UV and laser radiation

    International Nuclear Information System (INIS)

    Cuba, V.; Pavelkova, T.; Barta, J.; Indrei, J.; Gbur, T.; Pospisil, M.; Mucka, V.; Docekalova, Z.; Zavadilova, A.; Vlk, M.

    2011-01-01

    Complete text of publication follows. Radiation methods represent powerful tool for synthesis of various inorganic materials. Study of solid particles formation from solutions in the field of UV or ionizing radiation is one of the very promising and long term pursued trends in photochemistry and radiation chemistry. The motivation may be various, either preparation of new materials or removal of hazardous contaminants (e.g. heavy metals) from wastewater. This work deals with preparation of some metal oxides, synthetic garnets and spinel structures via irradiation of aqueous solutions containing precursors, i.e. soluble metal salts, radical scavengers and/or macromolecular stabilizers. Namely, results on radiation induced preparation of nickel, zinc, yttrium and aluminium oxides are summarized, as well as zinc peroxide, yttrium / lutetium - aluminium garnets and cobalt(II) aluminate. 60 Co irradiator, linear electron accelerator, medium pressure UV lamp and solid state laser were used as the sources of radiation. Aside from preparation, various physico-chemical and structural properties of compounds prepared were also studied. All used modifications of radiation method are rather convenient and simple, and yield (nano)powder materials with interesting characteristics. Prepared materials generally have high chemical purity, high specific surface area and narrow distribution of particles size (ranging in tens of nm). Generally, all types of irradiation result in materials with comparable properties and structural characteristics; but in the case of synthetic garnets and spinels, preparation using UV-radiation seems to be the most convenient for their preparation. Among compounds discussed, only zinc oxide and zinc peroxide were prepared directly via irradiation. For preparation of other crystalline compounds, additional heat treatment (at low temperature) of amorphous solid phase formed under irradiation was necessary.

  12. Preparation and characterization of thick BSCCO 2223 films

    International Nuclear Information System (INIS)

    Ciancio, G; Avila, A; Malachevsky, M.T; Ovidio, C.A

    2002-01-01

    Among the most widespread applications for critical high-temperature ceramic superconductors are for silver veined tapes, with the superconductor in the middle. These tapes are prepared by the powder- in - tube method. To attain high densities of critical current, the ceramic material must have a certain texture, with the grains oriented with the c axis perpendicular to the direction in which the current circulates. In the system that was studied, the degree of orientation increases as the distance to the vein decreases, with the maximum being in the silver-ceramic inter-phase. Superconductor tapes become inconvenient when defining the ceramic, especially because of the orientation of their plates as a function of the distance to the silver. Although the silver can be dissolved by a chemical attack in order to uncover the ceramic, greater precaution is needed while manipulating the superconductor and obtaining representative data. The behavior of thick films of the compound BSCCO 2223, deposited on silver sheets, forming silver-ceramic composites, was studied. These sheets simulate the silver-ceramic inter-phase and the distribution of the grains towards the center in a thick tape. After the samples were prepared, the phases that were present were characterized by x-ray diffraction and the resulting microstructure was analyzed with a SEM (Scanning Electron Microscope). Its mechanical properties were evaluated, following the formation and propagation of cracks in real time using four point flexion microassays inside the SEM chamber, as well as generating tension-deformation curves. The method of preparation of the thick films is discussed and its influence on the results obtained with the different characterizations (cw)

  13. Phases definition in marketing export process

    OpenAIRE

    Rajković Dragan; Kokić Miljko

    2004-01-01

    The result of export marketing process depends on its five phases. The first phase-revision of export capacities, inner view on advantages and defects of company concerning export possibilities. The second phase-identification of export strategy market penetration. The forth phase-preparing for the marketing campaign (action). The fifth phase-carrying out the above mentioned activities. This study shows the structure and contents of the mentioned phases. At the end, export marketing analyzed ...

  14. Representative Sampling for reliable data analysis

    DEFF Research Database (Denmark)

    Petersen, Lars; Esbensen, Kim Harry

    2005-01-01

    regime in order to secure the necessary reliability of: samples (which must be representative, from the primary sampling onwards), analysis (which will not mean anything outside the miniscule analytical volume without representativity ruling all mass reductions involved, also in the laboratory) and data...

  15. Preparation of tritium-labelled dextran and inulin

    International Nuclear Information System (INIS)

    Akulov, G.P.; Kaminski, Ju.L.; Korsakova, N.A.; Kudelin, B.K.

    1992-01-01

    Tritiated dextran and inulin were prepared by both a catalytic solid state and a liquid phase isotropic exchange with gaseous tritium. The liquid phase procedure is convenient for preparation of the polysaccharides with specific activities up to 5 mCi/g, while the solid state procedure allows specific activities up to 700 mCi/g. (Author)

  16. Steering committee for the management of the post-accidental phase of a nuclear accident or of a radiological situation (CODIRPA). Guidelines for the preparation to long term management of contaminated territories after a nuclear accident on the French territory - September 2012. Work document

    International Nuclear Information System (INIS)

    2012-09-01

    This publication aims at helping actors who want to be prepared to consider issues which would be raised by a post-accidental situation, at identifying economic, ecological and social vulnerabilities, notably local activities which might be impacted, even stopped, by a contamination of the environment. It discusses the situation assessment at the beginning of the long term phase, identifies governing principles for the post-accidental management on the long term. Then, it addresses the residence issue: to stay or to leave, to understand the situation or to be able to cope with radioactivity in everyday life, to care about one's health. The next addressed issues are work and production: identification of economic activity vulnerabilities, definition of a territory of project, adaptation of working conditions, re-deployment of activities and improvement of product radiological quality. The last part contains a set of proposals for a deeper preparation

  17. 14 CFR 1274.906 - Designation of New Technology Representative and Patent Representative.